Methods For Improving Skin Quality

ABSTRACT

A skin treatment regimen for delivery of a rinse-off personal skin care composition is provided. The rinse-off personal skin care composition includes varying ratios of a lathering agent to a hydrophobic benefit agent. The rinse-off personal skin care composition can be applied to skin of a user in phases over and/or in a treatment cycle. Each of the phases of the treatment cycle can include a ratio of the varying ratios that can be different such as higher or lower than a ratio of adjacent phase.

CROSS REFERENCE TO RELATED APPLICATION

This application claims the benefit of U.S. Provisional Application No. 61/295,732, filed Jan. 17, 2010 and U.S. Provisional Application No. 61/295,826, filed Jan. 18, 2010.

FIELD OF THE INVENTION

The present invention relates to methods for improving skin quality by delivering personal care articles that provide a premium product usage experience for the consumer and skin benefits that persist beyond the application.

BACKGROUND OF THE INVENTION

Personal care articles are well known and widely used on hair and skin for delivering actives that provide, for example, one or more benefits of cleansing, moisturizing, hiding or reducing imperfections, reducing oiliness, and providing scent to either or both the shower and the hair or skin. The efficacy of personal care compositions for cleaning and moisturizing, particularly with respect to reliving skin dryness and signs of aging, is directly related to the frequency of use and the level of benefit materials. And the pleasurable experience of using personal care compositions, particularly for the benefits of lathering and scenting, are similarly related to the frequency of use and the level of benefit materials in the personal care article.

Consumers typically have limited space to accommodate an extensive selection of personal care articles, hence they seek products that deliver the maximum benefits and pleasurable experience during use. If a treatment regime contains too many steps or too many packages, consumers often tire of the regime of personal care compositions over time. Likewise, if a personal care article contains a balance of actives that are perceived by consumers to provide an overall non-pleasurable usage experience, the consumers lose interest in using the product. As a result, in either case, consumer may decrease, suspend, or even or abandon use of the personal care article despite what may be significant benefits gained by the continued compliant use over time.

The methods of the present invention fulfill this need for a simplified regime that provides excellent skin benefits.

SUMMARY OF THE INVENTION

The present invention is directed to methods and regimens for application of a rinse-off personal care product for treating and maintaining the quality of skin and to minimize the signs of aging. Thus, in various embodiments, provided are skin treatment regimens that comprise applying to the skin of a user a composition formulated to comprise varying ratios of lathering agent to hydrophobic benefit agent, said varying ratios being either continuous or discrete in a treatment cycle comprising at least first and second phases. The composition applied during the first phase comprises a first of the varying ratios, and the composition applied during the second phase comprises a second of the varying ratios. In some embodiments, said second ratio is lower than the first ratio. In some embodiments, the treatment cycle comprises a third phase, and the composition applied therein comprises a third of the varying ratios. In some embodiments, said third ratio higher than the second ratio. In some embodiments, the composition is provided to the user through a delivery article adapted to dispense the composition in discrete aliquots of approximately equal volume.

The present invention is also directed to method of identifying and providing personal care products that are suitable for treating and maintaining the quality of skin. In some aspects the methods are directed to optimizing personal care products for specific populations of users.

The present invention is also directed to compositions and methods for assessing, treating and maintaining the quality of skin and minimizing the signs of aging by assessing the activity of one more skin biomarkers that are indicative of skin quality.

The regimens and methods of the present invention can be practiced using personal care articles for dispensing a personal care composition as disclosed herein. The disclosed personal care article comprises a single chamber package and a personal care article. The single chamber package comprises a dispensing orifice, a first zone proximal to the dispensing orifice, a second zone medial to the dispensing orifice, and a third zone distal to the dispensing orifice. The personal care article comprises a first personal care composition, a second personal care composition and a third personal care composition. The first personal care composition is substantially within the first zone and comprises a first concentration of a hydrophobic benefit material. The second personal care composition is substantially within the second zone and comprises a second concentration of a hydrophobic benefit material. The third personal care composition is substantially within the third zone and comprises a third concentration of a hydrophobic benefit material. The second concentration is greater than the first concentration and the third concentration of the hydrophobic benefit material.

In another aspect of the present invention, the first concentration comprises from about 15% to less than 35%, by weight of the first personal care composition, of hydrophobic benefit material, the second concentration comprises from about 35% to about 65%, by weight of the second personal care composition, of hydrophobic benefit material, and the third concentration comprises from about 15% to less than 35%, by weight of the third personal care composition, of hydrophobic benefit material. The first personal care composition is capable of being substantially dispensed prior to the second and third personal care composition. The second personal care composition is capable of being substantially dispensed prior to the third personal care composition.

These and other features, aspects, and advantages of the present invention will become evident to those skilled in the art from a reading of the present disclosure with the appended claims.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1A and FIG. 1B illustrate a personal care article with three zones having horizontal interfaces between the compositions in each zone.

FIG. 2A is a diagram of the distinguishable layers of a personal care product after centrifugation which can be measured in length to calculate the concentration of hydrophobic benefit material in the personal care product using the Microcentrifugation Method described below.

FIG. 2B and FIG. 2C are photographs that exemplify the measurement of the length of the benefit layer used to calculate the concentration of the hydrophobic benefit material within in centrifuged samples tested using the Microcentrifugation Method described below.

FIG. 3 is a calibration curve calculated using a formula in the Microcentrifugation Method described below.

FIG. 4 illustrates a graphic user interface analysis a personal care product phase distribution along the radial dimensions of the package according to the MRI method described below.

FIG. 5 illustrates a graphic user interface analysis of a personal care product phase distribution along the height of the package according to the MRI method described below.

FIG. 6A, FIG. 6B, and FIG. 6C are MRI images of hydrophobic benefit material distribution profiles prior to and after simulated shipping conditions, as per the Dynamic Stability Shipping Method described below.

FIG. 7A, FIG. 7B and FIG. 7C are MRI images of hydrophobic benefit material distribution profiles of personal care products described in the examples below.

FIG. 8 is a chart showing the benefit phase distribution profile of the hydrophobic benefit material in the personal care products described in the examples below.

An appendix of figures is also provided, and includes:

FIG. 9 is a chart showing the lipid delivery profile according to an embodiment as described herein wherein the ratio of lathering agent to hydrophobic benefit agent varies across a treatment cycle from about 70:30 through about 45:55 to about 80:20.

FIG. 10 is a graph showing the relative change in visual dryness using water and a embodiment of personal care composition having the lipid delivery profile as shown in FIG. 9.

FIG. 11 is a graph showing the relative change in skin condition measured with a corneometer using water and a embodiment of personal care composition having the lipid delivery profile as shown in FIG. 9.

FIG. 12 is a graph showing the relative change in skin trans epidermal water loss using water and a embodiment of personal care composition having the lipid delivery profile as shown in FIG. 9.

FIG. 13 is a graph showing the relative change in visual dryness using water, a personal care composition having a lathering agent to hydrophobic benefit agent ratio of 44:45 and a embodiment of personal care composition having the lipid delivery profile as shown in FIG. 9.

FIG. 14 is a graph showing the relative change in skin condition measured with a corneometer using water, a personal care composition having a lathering agent to hydrophobic benefit agent ratio of 44:45 and a embodiment of personal care composition having the lipid delivery profile as shown in FIG. 9.

FIG. 15 is a graph showing the relative change in skin trans epidermal water loss using water, a personal care composition having a lathering agent to hydrophobic benefit agent ratio of 44:45 and a embodiment of personal care composition having the lipid delivery profile as shown.

FIG. 16 is a graph showing the change in skin deformation over time.

FIG. 17 is a graph showing the relative change in Ue using water and a embodiment of personal care composition having the lipid delivery profile as shown in FIG. 9.

FIG. 18 is a graph showing the relative change in Ur using water and a embodiment of personal care composition having the lipid delivery profile as shown in FIG. 9.

FIG. 19 is a graph showing the relative change in Ue using water, a personal care composition having a lathering agent to hydrophobic benefit agent ratio of 44:45 and a embodiment of personal care composition having the lipid delivery profile as shown in FIG. 9.

FIG. 20 is a graph showing the relative change in Ur using water, a personal care composition having a lathering agent to hydrophobic benefit agent ratio of 44:45 and a embodiment of personal care composition having the lipid delivery profile as shown in FIG. 9.

FIG. 21 is a graph showing the relative change in total protein using water and a embodiment of personal care composition having the lipid delivery profile as shown in FIG. 9

FIG. 22 is a graph showing the relative change in total protein using water, a personal care composition having a lathering agent to hydrophobic benefit agent ratio of 44:45 and a embodiment of personal care composition having the lipid delivery profile as shown in FIG. 9

FIG. 23 is a graph showing the relative change in Keratin 1, 10 and 11 normalized to soluble protein using water and a embodiment of personal care composition having the lipid delivery profile as shown in FIG. 9

FIG. 24 is a graph showing the relative change Keratin 1, 10 and 11 normalized to soluble protein using water, a personal care composition having a lathering agent to hydrophobic benefit agent ratio of 44:45 and a embodiment of personal care composition having the lipid delivery profile as shown in FIG. 9.

FIG. 25 is a graph showing the lipid delivery profile according to an embodiment as described herein wherein the ratio of lathering agent to hydrophobic benefit agent varies across a treatment cycle from about 70:30 through about 45:55 to about 80:20, wherein the volume of dispensed composition is 250 ml.

FIG. 26 is a graph showing the lipid delivery profile according to an embodiment as described herein wherein the ratio of lathering agent to hydrophobic benefit agent varies across a treatment cycle from about 70:30 through about 45:55 to about 80:20, wherein the volume of dispensed composition is 450 ml.

DETAILED DESCRIPTION OF THE INVENTION I. Definitions

“Ambient conditions” as used herein, refers to surrounding conditions at one (1) atmosphere of pressure, 50% relative humidity, and 25° C.

“Biomarker” as used herein refers to any biological molecules (genes, proteins, lipids, metabolites) that, singularly or collectively, reflect the current or predict future state of a biological system. Thus, as used herein, various biomarkers are indicators of the quality of skin in terms of elasticity, dryness, condition, brightness, tone, smoothness, appearance of lines. Non-limiting examples of biomarkers include, elastic properties, visual properties of dryness and condition, the presence of flaking, cohesiveness as evidenced by total protein, lipid content, trans epidermal water loss, cytokine expression, the presence of one or more of keratins 1, 10 and 11. One or more modified biological parameters can be used to screen for materials that induce a positive or negative effect on skin. The response of skin to treatment with personal care compositions can also be assessed by measuring one or more biomarkers.

“Comprising” as used herein means that other steps and other ingredients which do not affect the end result can be added. This term encompasses the terms “consisting of” and “consisting essentially of.” The compositions and methods/processes of the present invention can comprise, consist of, or consist essentially of the essential elements and limitations of the invention described herein, as well as any of the additional or optional ingredients, components, steps, or limitations described herein useful in personal cleansing compositions intended for topical application to the hair or skin.

“Effective amount” as used herein means an amount of a compound or composition sufficient to significantly induce a positive skin benefit, including independently or in combination with other benefits disclosed herein. This means that the content and/or concentration of active component in the formulation is sufficient that when the formulation is applied with normal frequency and in a normal amount, the formulation can result in the treatment of one or more undesired skin conditions (e.g., skin wrinkles). For instance, the amount can be an amount sufficient to inhibit or enhance some biochemical function occurring within the skin. This amount of active component may vary depending upon the type of product, the type of skin condition to be addressed, and the like.

“Headspace,” as used herein means the void volume that is located proximal to the dispensing orifice and the interface of the first zone of the single chamber package. In the alternative, the headspace can be comprised within the first zone. The headspace of the personal care articles of the present invention can be determined by the following method or any other conventional method. First, an empty package is placed on a balance and weighed. The total package volume is determined by completely filling the package with deionized water and determining the deionized water weight and recording it as (V_(total)). The package is then filled with a personal care composition leaving a headspace. Next, the package is placed on a balance and re-zero. The headspace volume is filled with deionized water by a syringe. The weight of deionized water filled in the headspace is recorded as (V_(headspace)). The headspace is calculated as: V_(headspace)/V_(total)*100%.

“Hydrophobic benefit agent” as used herein, refers to hydrophobic benefit materials that deliver skin conditioning, moisturization, and skin health benefits. Preferably, hydrophobic benefit agents are selected from the group consisting of petrolatum, lanolin, derivatives of lanolin (e.g. lanolin oil, isopropyl lanolate, acetylated lanolin, acetylated lanolin alcohols, lanolin alcohol linoleate, lanolin alcohol riconoleate) hydrocarbon oils (e.g. mineral oil) natural and synthetic waxes (e.g. micro-crystalline waxes, paraffins, ozokerite, lanolin wax, lanolin alcohols, lanolin fatty acids, polyethylene, polybutene, polydecene, pentahydrosqualene) volatile or non-volatile organosiloxanes and their derivatives (e.g. dimethicones, cyclomethicones, alkyl siloxanes, polymethylsiloxanes, methylphenylpolysiloxanes), natural and synthetic triglycerides (e.g. castor oil, soy bean oil, sunflower seed oil, maleated soy bean oil, safflower oil, cotton seed oil, corn oil, walnut oil, peanut oil, olive oil, cod liver oil, almond oil, avocado oil, palm oil, sesame oil) and combinations thereof.

“Liquid” as used herein means that the composition is generally flowable to some degree. “Liquids”, therefore, may include liquid, semi-liquid, cream, lotion or gel compositions intended for topical application to skin. The compositions may exhibit a viscosity of equal to or greater than about 1,500 (centipoise, hereinafter “cps”), equal to or greater than about 5,000 cps, equal to or greater than about 10,000 cps or equal to or greater than about 20,000 cps and no more than about 1,000,000 cps, no more than about 500,000 cps, no more than about 300,000 cps, or no more than about 200,000 cps as measured by the T-Bar Viscosity Method described hereinafter.

“Lathering Agent” as used herein refers to a surfactant, which when combined with water and mechanically agitated generates a foam or lather sufficient to cause a personal care composition to provide a lather.

“Package” includes any suitable container for personal care compositions exhibiting a viscosity from about 1,500 centipoise (cP) to about 1,000,000 cP, including but not limited to a bottle, tottle, tube, jar, non-aerosol pump and mixtures thereof.

“Personal care composition” as used herein, refers to compositions intended for topical application to the skin or hair. The compositions used in accordance with the present invention are rinse-off formulations, in which the product is applied topically to the skin or hair and then is subsequently rinsed within minutes from the skin or hair with water, or otherwise wiped off using a substrate with deposition of a portion of the composition. The compositions also may be used as shaving aids. The personal care composition used in accordance with the present invention is typically extrudable or dispensible from a single chamber package. The personal care compositions used in accordance with the present invention can be in the form of liquid, semi-liquid, cream, lotion or gel compositions intended for topical application to skin. Examples of personal care compositions used in accordance with the present invention can include but are not limited to shampoo, conditioning shampoo, hair conditioner, body wash, moisturizing body wash, shower gels, skin cleansers, cleansing milks, hair and body wash, in shower body moisturizer, pet shampoo, shaving preparations and cleansing compositions used in conjunction with or applied to a disposable cleansing cloth. The product forms contemplated for purposes of defining the compositions and methods of the present invention are rinse-off formulations by which it is meant that the product is applied topically to the skin or hair and then subsequently (i.e., within minutes) rinsed away with water, or otherwise wiped off using a substrate or other suitable removal means.

“Phase” as used herein refers to a distinguishable part in a cycle of treatment or application of a personal care product according to the invention. For purposes hereof, a phase need not be limited to a particular period of time. Phases are distinct from one another in that the properties, most particularly the ratios of lathering agent to hydrophobic benefit agent, of a personal care composition vary between sequential phases. Thus, in a cycle comprising three phases of treatment or application, each phase may involve use of personal care compositions that vary relative to one another, for example wherein the ratios of lathering agent to hydrophobic benefit agent vary between each of the phases. In another example, in a cycle comprising three phases of treatment or application, two of the phases may involve use of personal care compositions that do not vary relative to one another while a third phase varies from the other two. In yet another example in a cycle comprising two phases of treatment or application, each phase may involve use of personal care compositions that vary relative to one another, for example wherein the ratios of lathering agent to hydrophobic benefit agent vary between each of the phases. The terms “Premium Experience Phase” refers to phases in which the components in a personal care composition are associated with delivery of one or more experiential benefits to the user at the time of use, such as lathering and delivery of scent for excellent in-use characteristics during cleansing process. The term “Conditioning Phase” refers to phases in which the components in a personal care composition are associated with delivery of one or more benefits during use, for example, deposition of hydrophobic benefit agent on the skin, that provide long term benefits after use.

“Sagging” as used herein means the laxity, slackness, or the like condition of skin that occurs as a result of loss of, damage to, alterations to, and/or abnormalities in dermal elastin, muscle and/or subcutaneous fat.

“Signs of aging” include, but are not limited to, all outward visibly and tactilely perceptible manifestations as well as any other macro or micro effects due to skin aging. Such signs may be induced or caused by intrinsic factors or extrinsic factors, e.g., chronological aging and/or environmental damage. These signs may result from processes which include, but are not limited to, the development of textural discontinuities such as wrinkles and coarse deep wrinkles, fine lines, skin lines, crevices, bumps, large pores (e.g., associated with adnexal structures such as sweat gland ducts, sebaceous glands, or hair follicles), or unevenness or roughness, loss of skin elasticity (loss and/or inactivation of functional skin elastin), sagging (including puffiness in the eye area and jowls), loss of skin firmness, loss of skin tightness, loss of skin recoil from deformation, discoloration (including undereye circles), blotching, sallowness, hyperpigmented skin regions such as age spots and freckles, keratoses, abnormal differentiation, hyperkeratinization, elastosis, collagen breakdown, and other histological changes in the stratum corneum, dermis, epidermis, the skin vascular system (e.g., telangiectasia or spider vessels), and underlying tissues (e.g., fat and/or muscle), especially those proximate to the skin.

“Skin,” as used herein, refers to keratin-containing layers disposed as the outermost protective covering of mammals (e.g., humans, dogs, cats, etc.) which includes, but is not limited to, skin, mucosa, lips, hair, toenails, fingernails, cuticles, hooves, etc.

“Smoothing” and “softening” as used herein mean altering the surface of the skin such that its tactile feel is improved.

“Surfactant component” as used herein means the total of all anionic, nonionic, amphoteric, zwitterionic and cationic surfactants in a phase. When calculations are based on the surfactant component, water and electrolyte are excluded from the calculations involving the surfactant component, since surfactants as manufactured typically are diluted and neutralized.

“Statically stable” as used herein, unless otherwise specified, refers to a personal care article that comprise at least two compositions that maintain at least two “separate” zones with at least two separate benefit concentrations zones contained within a single chamber package at ambient conditions for a period of at least about 180 days. Alternatively, static stability can be determined by accelerated protocol at elevated temperature. One accelerated protocol is based on passing static stability after 10 days at 50° C. By “separate” is meant that there is substantially no mixing of compositions contained in the zones, detected by the benefit analysis method, described hereinafter, prior to dispensing of the composition.

“Structured,” as used herein means having a rheology that confers stability on the personal care composition. The degree of structure is determined by characteristics determined by one or more of the following methods the Yield Stress Method, or the Zero Shear Viscosity Method or by the Ultracentrifugation Method, all in the Test Methods below. Accordingly, a surfactant phase of the composition used in accordance with the present invention is considered “structured,” if the surfactant phase has one or more of the following properties described below according to the Yield Stress Method, or the Zero Shear Viscosity Method or by the Ultracentrifugation Method. A surfactant phase is considered to be structured, if the phase has one or more of the following characteristics:

A. a Yield Stress of greater than about 0.1 Pascal (Pa), more typically greater than about 0.5 Pa, even more typically greater than about 1.0 Pa, still more typically greater than about 2.0 Pa, still even more typically greater than about 3 Pa, and even still even more typically greater than about 5 Pa as measured by the Yield Stress and Zero Shear Viscosity Method described hereafter:

B. a Zero Shear Viscosity of at least about 500 Pascal-seconds (Pa-s), typically at least about 1,000 Pa-s, more typically at least about 1,500 Pa-s, even more typically at least about 2,000 Pa-s; or

C. a Structured Domain Volume Ratio as measured by the Ultracentrifugation Method described hereafter, of greater than about 40%, typically at least about 45%, more typically at least about 50%, more typically at least about 55%, more typically at least about 60%, more typically at least about 65%, more typically at least about 70%, more typically at least about 75%, more typically at least about 80%, even more typically at least about 85%.

“Topical application”, “topically”, and “topical”, as used herein, mean to apply (e.g., spread, spray) the compositions used in accordance with the present invention onto the surface of the skin.

“Tottle” as used herein refers to a bottle which rests on the neck or mouth which its contents are filled in and dispensed from, but it is also the end upon which the bottle is intended to rest or sit upon for storage by the consumer and/or for display on the store shelf, as described in the commonly owned U.S. patent application Ser. No. 11/067,443 filed on Feb. 25, 2005 to McCall et al, entitled “Multi-phase Personal Care Compositions, Process for Making and Providing, and Article of Commerce.”

“Treating” or “treatment” or “treat” as used herein includes regulating and/or immediately improving skin cosmetic appearance and/or feel. As used herein, “regulating” or “regulation” means maintaining or improving the health and/or cosmetic appearance, and includes both prophylactically regulating and/or therapeutically regulating. Regulation of skin condition, namely mammalian and in particular human skin, hair, or nail condition, is often required due to conditions which may be induced or caused by factors internal and/or external to the body. Examples include environmental damage, radiation exposure (including ultraviolet radiation), chronological aging, menopausal status (e.g., post-menopausal changes in skin, hair, or nails), stress, diseases, disorders, etc. For instance, “regulating skin, hair, or nail condition” includes prophylactically regulating and/or therapeutically regulating skin, hair, or nail condition, and may involve one or more of the following benefits: thickening of skin, hair, or nails (e.g., building the epidermis and/or dermis and/or sub-dermal [e.g., subcutaneous fat or muscle] layers of the skin, and where applicable the keratinous layers of the nail and hair shaft) to reduce skin, hair, or nail atrophy, increasing the convolution of the dermal-epidermal border (also known as the rete ridges), preventing loss of skin or hair elasticity (loss, damage and/or inactivation of functional skin elastin) such as elastosis, sagging, loss of skin or hair recoil from deformation; melanin or non-melanin change in coloration to the skin, hair, or nails such as under eye circles, blotching (e.g., uneven red coloration due to, e.g., rosacea) (hereinafter referred to as “red blotchiness”), sallowness (pale color), discoloration caused by telangiectasia or spider vessels, and graying hair.

“Zone” as used herein refers to a domain or region within a single chamber package which corresponds to a composition of the personal care article. The interface between the zones can be distinct or gradual or separated by another zone. The amount contained within a zone can be defined by a percentage of the package volume and a zone comprises at least 10% of the package volume of a given package, excluding the volume of the package corresponding to the necessary headspace or void volume and the closure, as shown in FIG. 1A and FIG. 1B of the present invention. In one aspect, the first personal care composition, the second personal care composition and third personal care compositions within a the first zone, second zone or third zone is homogeneous. In this case, the concentration of hydrophobic benefit material is constant within the zone. In another aspect, the personal care composition within the first, second or third zone is inhomogeneous, such that the concentration of hydrophobic benefit material varies within the zone. The level of hydrophobic benefit material can show an increasing or decreasing trend.

All percentages, parts and ratios are based upon the total weight of the compositions used in accordance with the present invention, unless otherwise specified. All such weights as they pertain to listed ingredients are based on the active level and, therefore; do not include solvents or by-products that may be included in commercially available materials, unless otherwise specified. The term “weight percent” may be denoted as “wt. %” herein. Except where specific examples of actual measured values are presented, numerical values referred to herein should be considered to be qualified by the word “about.”

All molecular weights as used herein are weight average molecular weights expressed as grams/mole, unless otherwise specified.

II. Methods and Regimens for Treating Skin

The personal care compositions used in accordance with the present invention are used in a conventional manner for cleansing and conditioning skin. The personal care compositions used in accordance with the present invention are typically applied topically to the desired area of the skin in an amount sufficient to provide effective delivery of the skin cleansing agent, hydrophobic material, and in some embodiments particles and other agents and actives to the applied surface. The compositions can be applied directly to the skin or indirectly via the use of a cleansing puff, washcloth, sponge or other implement. The compositions are typically diluted with water prior to, during, or after topical application, and then subsequently the skin is rinsed or wiped off, typically rinsed off of the applied surface using water or a water-insoluble substrate in combination with water.

The present invention is therefore also directed to methods of cleansing the skin through the above-described application of the compositions of the present invention. An effective amount of the composition for cleansing and conditioning the skin is applied to the skin, that in some examples has been wetted with water, and then rinsed off. Such effective amounts generally range from about 1 gm to about 50 gm, and from about 1 gm to about 20 gm.

In general, a typical method for cleansing and conditioning the skin comprises the steps of: a) wetting the skin with water, b) applying an effective amount of the personal care composition to the skin, and c) rinsing the applied areas of skin with water. These steps can be repeated as many times as desired to achieve the desired cleansing and conditioning benefit.

Treatment Regimens

In various embodiments, the invention provides methods and regimens for use of a personal care composition having varied ratios of lathering agent to hydrophobic benefit agent. The composition is used over a period of time, alternately referred to as a treatment time, that includes two or more phases. In some embodiments, the treatment period includes three phases, starting with first phase in which a high lathering agent (surfactant) is used that provides a premium user experience through high lather and fragrance delivery. According to such embodiments, as use progresses into a second phase, a high lipid “plateau” provides conditioning through high hydrophobic benefit agent content, and in a final phase a high lathering agent (surfactant) is used that provides a premium user experience through high lather and fragrance delivery. In other embodiment, the order of the phases may be switched and a treatment period may comprise only two phases, or it may comprise more than three phases.

In various embodiments, skin treatment regimens are provided comprising (i) providing to a user a composition formulated to comprise varying ratios of lathering agent to hydrophobic benefit agent, said varying ratios being either continuous or discrete; and (ii) applying the provided composition to the skin of the user in a treatment cycle comprising at least first and second phases. The composition applied during the first phase comprises a first of the varying ratios, and the composition applied during the second phase comprises a second of the varying ratios. In some embodiments, said second ratio is lower than the first ratio. In some embodiments, the treatment cycle comprises a third phase, and the composition applied therein comprises a third of the varying ratios. In accordance with the invention, provided are regimens for the delivery of a rinse-off personal skin care composition. Some embodiments include the steps of dispensing from a personal care article a personal care composition that comprises a lathering agent and a hydrophobic benefit agent, wherein the article operates to dispense the composition in aliquots, and wherein the ratio of lathering agent to hydrophobic benefit agent varies in successively dispensed aliquots of the composition over the course of dispensing the article contents such that the amount of hydrophobic benefit agent in two or more successive aliquots is different. According to such embodiments, the steps include applying a first aliquot of the personal care composition to a user's skin together with water, wherein the lathering agent provides lather when contacted on the user's skin with water and rinsing the personal care composition from the user's skin, wherein a portion of the hydrophobic benefit agent is deposited and remains on the user's skin after rinsing.

In accordance with some embodiments of the regimens, the steps include: application of a composition to skin of a user in phases over a treatment cycle. It will be understood that a treatment cycle is described herein as been achieved in phases, however, the term phrases is intended to be non-limiting with respect to time or sequence of the steps of a treatment cycle. In the various embodiments, the composition comprises varying ratios of a lathering agent to a hydrophobic benefit agent. A treatment cycle includes a first phase characterized by the application of the composition having a first ratio of the varying ratios, an intermediate phase characterized by the application of the composition having a second ratio of the varying ratios that is lower than the first ratio, and a final phase characterized by the application of the composition having a third ratio of the varying ratios that is higher than the intermediate phase.

The invention also provides regimens for sustaining consumer use of a treatment for skin. In various embodiments, the regimen involves application of the composition to a user's skin in a treatment cycle having a first phase wherein the ratio of lathering agent to hydrophobic benefit agent is high and provides a relatively appealing sensation to the consumer, an intermediate phase wherein the ratio of lathering agent to hydrophobic benefit agent is low and provides a relatively less appealing sensation to the consumer, and a final phase wherein the ratio of lathering agent to hydrophobic benefit agent is high and provides a relatively appealing sensation to the consumer.

The invention also provides regimens for maintaining the quality of skin with a rinse-off personal care composition which include the steps of applying the composition to a user's skin on a daily basis for a period of days, wherein the composition is a rinse-off personal skin care composition comprising a hydrophobic benefit agent and a lathering agent, and wherein the ratio of lathering agent to hydrophobic benefit agent varies over the period of application, the period of days of application comprising, in any order, a premium experience phase wherein the ratio of lathering agent to hydrophobic benefit agent is high, the premium experience phase characterized by maximal delivery of lather and scent, and a conditioning phase wherein the ratio of lathering agent to hydrophobic benefit agent is low, the conditioning phase characterized by maximal hydrophobic benefit agent deposition. In some embodiments the sequence of the phases is the premium experience phase followed by the conditioning phase. In other embodiments, the sequence of the phases is the conditioning phase followed by the premium experience phase. In yet other embodiments, the sequence of the phases is a premium experience phase, followed by a conditioning phase, followed by a premium experience phase.

In some embodiments, said third ratio higher than the second ratio. In some embodiments, the composition is provided to the user through a delivery article adapted to dispense the composition in discrete aliquots of approximately equal volume. In some embodiments, the composition comprises a continuum of varying ratios, and at least every other aliquot provided to the user has a different ratio of lathering agent to hydrophobic benefit agent. In some embodiments, every aliquot provided to the user has a different ratio. In some embodiments, at least every other aliquot provided and applied during the first phase has a lower ratio of lathering agent to hydrophobic benefit agent.

In accordance with some embodiments, the composition is provided in a delivery article that contains sufficient composition for at least one treatment cycle. According to such embodiments, the delivery article is adapted to dispense the composition in discrete aliquots of approximately equal volume, and wherein aliquots of the composition are applied until the contents of the delivery article are substantially depleted. In some embodiments the each aliquot has the same approximate volume. In some embodiments the volume of each successively dispensed aliquot increases. In some embodiments a first dispensed aliquot comprises a first ratio of the varying ratios, and a subsequent dispensed aliquot comprises a second ratio of the varying ratios that is different from the ratio of the first aliquot. According to such embodiments, an aliquot dispensed subsequent to the second aliquot comprises a third ratio of the varying ratios that is different from the ratio of the second aliquot. In some embodiments, an aliquot dispensed subsequent to the second aliquot comprises a third ratio of the varying ratios that is different from the ratio of the first aliquot. In some embodiments an aliquot dispensed subsequent to the second aliquot comprises a third ratio of the varying ratios that is different from the ratios of the first and the second aliquots.

Suitable aliquots for application during the first phase include, but are not limited to, those having a ratio of lathering agent to hydrophobic benefit agent from about 90:10 to about 50:50. Accordingly, non-limiting examples of suitable aliquots for application during the first phase are those having ratios of 90:10, 85:15, 80:20, 75:25, 70:30, 65:35, 60:40, 55:45, and 50:50. In some embodiments, at least every other aliquot provided and applied during the second phase has a lower ratio of lathering agent to hydrophobic benefit agent. Suitable aliquots for application during the second phase include, but are not limited to, those having a ratio of lathering agent to hydrophobic benefit agent from about 50:50 to about 10:90.

Accordingly, non-limiting examples of suitable aliquots for application during the second phase are those having ratios of 50:50, 45:55, 40:60, 35:65, 30:70, 25:75, 20:80, 15:85, and 10:90. In some embodiments, at least every other aliquot applied during the third phase has a higher ratio of lathering agent to hydrophobic benefit agent. Suitable aliquots for application during the third phase include, but are not limited to, those having a ratio of lathering agent to hydrophobic benefit agent from about 50:50 to about 90:10. Accordingly, non-limiting examples of suitable aliquots for application during the third phase are those having ratios of 50:50, 55:45, 60:40, 65:35, 70:30, 75:25, 80:20, 85:15, and 90:10.

In some embodiments, the composition comprises discrete varying ratios, and each aliquot provided to the user during a phase has the same ratio of lathering agent to hydrophobic benefit agent. For example, the composition may be in discrete zones within the delivery article, each zone having a different ratio of lathering agent to hydrophobic benefit agent. As further example, each zone may correspond to a phase of the treatment regimen. In the embodiments wherein the composition comprises discrete ratios of lathering agent to hydrophobic benefit agent, suitable aliquots for application during the first phase include, but are not limited to, those having a ratio from about 90:10 to about 50:50. Accordingly, non-limiting examples of suitable aliquots for application during the first phase are those having ratios of 90:10, 85:15, 80:20, 75:25, 70:30, 65:35, 60:40, 55:45, and 50:50.

In the embodiments wherein the composition comprises discrete ratios of lathering agent to hydrophobic benefit agent, suitable aliquots for application during the second phase include, but are not limited to, those having a ratio from about 50:50 to about 10:90. Accordingly, non-limiting examples of suitable aliquots for application during the second phase are those having ratios of 50:50, 45:55, 40:60, 35:65, 30:70, 25:75, 20:80, 15:85, and 10:90. In the embodiments wherein the composition comprises discrete ratios of lathering agent to hydrophobic benefit agent, suitable aliquots for application during the third phase include, but are not limited to, those having a ratio from about 50:50 to about 90:10. Accordingly, non-limiting examples of suitable aliquots for application during the third phase are those having ratios of 50:50, 55:45, 60:40, 65:35, 70:30, 75:25, 80:20, 85:15, and 90:10.

In accordance with some embodiments, the composition is applied on a daily basis. It will be appreciated that treatment times and frequency may vary based upon the user, and as such, treatment may be on a less than daily basis, or may be more often. In other embodiments, the treatments may be less frequent, for example weekly or monthly, or in some other interval of time.

In accordance with the methods, the composition is provided in a delivery article that is adapted for use in accordance with a predetermined time of treatment or a predetermined approximate number of instances of treatment, or both. Thus, in some embodiments, the delivery article is adapted to deliver sufficient composition for one or two or more treatment cycles. In some embodiments, the delivery article is adapted to deliver the composition for each treatment cycle in an approximate number of aliquots or units. In such embodiments, the aliquots may be the same in volume or may vary. In some embodiments the number of aliquots or units to be dispensed per phase or in an article is a predetermined number that defines the approximate number of instances of use, either in days, weeks or months.

In some embodiments the composition is applied through a treatment cycle in a time interval of about thirty days. For example, the first phase of the treatment cycle may be from about 3 to 7 days, the intermediate phase of the treatment cycle may be from about 6 to 14 days, and the final phase of the treatment cycle may be from about 6 to 14 days. In another example, the first phase of the treatment cycle may be from about 2 to 5 days, the intermediate phase of the treatment cycle may be from about 3 to 7 days, and the final phase of the treatment cycle may be from about 14 to 21 days.

In another embodiment, the composition is applied through a treatment cycle in a time interval of about fifty days. In one example, the first phase of the treatment cycle may be from about 3 to 7 days, the intermediate phase of the treatment cycle may be from about 10 to 28 days, and the final phase of the treatment cycle may be from about 14 to 20 days.

In another embodiment, the applied through a treatment cycle in a time interval of about fifty-six days. In one example, the first phase of the treatment cycle may be from about 2 to 7 days, the intermediate phase of the treatment cycle may be from about 3 to 28 days, and the final phase of the treatment cycle may be from about 6 to 21 days

In accordance with various embodiments, the ratios of lathering agent to hydrophobic benefit agent may vary in each phase across a broad possible range. In some embodiments, the ratio of lathering agent to hydrophobic benefit agent is at a maximum of about 75:25 during the first phase, and the ratio of lathering agent to hydrophobic benefit agent is at a minimum of about 45:55 during the intermediate phase, and the ratio of lathering agent to hydrophobic benefit agent is at a maximum of about 75:25 during the final phase. In other embodiments, the ratio of lathering agent to hydrophobic benefit agent is at a maximum of about 70:30 during the first phase, and the ratio of lathering agent to hydrophobic benefit agent is at a minimum of about 45:55 during the intermediate phase, and the ratio of lathering agent to hydrophobic benefit agent is at a maximum of about 80:20 during the final phase. In yet other embodiments, the ratio of lathering agent to hydrophobic benefit agent is at a maximum of about 75:25 during the first phase, and the ratio of lathering agent to hydrophobic benefit agent is at a minimum of about 45:55 during the intermediate phase, and the ratio of lathering agent to hydrophobic benefit agent is at a maximum of about 75:25 during the final phase. In some general embodiments, the ratio of lathering agent to hydrophobic benefit agent is at a maximum in the range from about 50:50 to 90:10 during the first phase, and the ratio of lathering agent to hydrophobic benefit agent is at a minimum in the range from about 10:90 to 50:50 during the intermediate phase, and the ratio of lathering agent to hydrophobic benefit agent is at a maximum in the range from about 50:50 to 90:10 during the final phase.

It will be appreciated that the variations in ratios in each phase and between the phases may vary independently of the interval time of treatment, and that the number of days of treatment during any phase in a described interval may vary. Further, it will be appreciated that the number of aliquots or units of composition dispensed or used in a treatment cycle, during any phase, or in any single application may vary, and that the volume of aliquots may vary.

In accordance with some embodiments, a delivery article is adapted to deliver composition formulated to match a population profile, wherein the profile reflects preferences in a population for composition properties selected from maximum hydrophobic benefit agent content, lathering, scent, color, opalescence, thickness, and combinations of these. Methods of identifying population profiles and developing personal care compositions are described herein.

In accordance with various embodiments, the composition formulation used in accordance with the methods may include one or more additional benefit agents. Non limiting examples of benefit agents includes vitamins, vitamin derivatives, sunscreens, desquamation actives, anti-wrinkle actives, anti-atrophy actives, anti-oxidants, skin soothing agents, skin healing agents, skin lightening agents, skin tanning agents, anti-acne medicaments, essential oils, sensates, pigments, colorants, pearlescent agents, interference pigments, particles, hydrophobically modified non-platelet particles and combinations thereof. Other benefit agents and materials as described herein with respect to representative composition embodiments may also be used. Likewise, other formulation components, including lathering/surfactant agents and hydrophobic benefit agents may be selected as described herein. Additional benefit agents may be provide with either or both the lathering agent and the hydrophobic benefit agent. Examples of some specific benefit agents include exfoliating agents, niacinamide, vitamin E (tocopherol or tocotrieneol), collagen.

According to the various embodiments, personal care compositions provide a lathering agent that produces a lather that varies with the varied ratios of lathering agent and hydrophobic benefit agent. In some embodiments the lather volume of the composition is greater than from about 800 ml to 1500 ml by the cylinder lather method. It will thus be appreciated by those in the art that in accordance with the cylinder method, the lather volume provided by a personal care composition may be from about 800, 850, 900, 950, 1000, 1050, 1100, 1150, 1200, 1250, 1300, 1350, 1400, 1450, and 1500 or more ml. Of course it will be appreciated that in some embodiments, particular with respect to embodiments and phases wherein the ratio of lathering agent to hydrophobic benefit agent is low, that the lather volume will be lower or substantially lower than the above stated range, and that in some embodiments the lather volume may be from 1500 to 1750 to 1900, to 2000 or more ml. It will also be appreciated that other methods described or otherwise known in the art may be used to characterize lather and lather volume and that the description herein is not limiting, such that the lather properties of the compositions used as described herein may be described in other terms.

In accordance with varying embodiments, the methods and regimens involve the use of personal care compositions provided in one or more delivery articles. In some embodiments the ratios of the lathering agent to hydrophobic benefit agent in the composition vary as a function of containment location in the single delivery article. In some embodiments the composition is contained within discrete zones of the delivery article and wherein ratios of lathering agent to hydrophobic benefit agent are different in each zone. According to such embodiments, the discrete zones are physically separated chambers defined in the delivery article. In some embodiments the personal care composition is provided in a delivery article adapted to dispense the composition in discrete aliquots of approximately equal volume. In some such embodiments, the delivery article contains sufficient composition for a predetermined application period. In some embodiments aliquots of the composition are dispensed and applied until the contents of the delivery article are substantially depleted

In some embodiments the ratios of the lathering agent to hydrophobic benefit agent in the composition vary continuously from the first phase through the final phase. It will be appreciated that the variation across a phase or phases may be influenced by the volume increments of composition provided. In some embodiments, two or more sequential increments of provided composition may be the same with respect to the ratios of lathering agent to hydrophobic benefit agent. In other embodiments, each increment may be the same.

According to some embodiments, the quality of the users skin after the conditioning phase exhibits improvement sufficient to be detected by measurement of one or more of reduction of visual dryness, reduction in trans-epidermal water loss, increased skin hydration, increased elastic extension, increased elastic recovery, increased firmness, reduction in total protein, increase in the amount of one or more of Keratin 1, Keratin 10 and Keratin 11, and decrease in cytokine expression. According to some embodiments the quality of the users skin is maintained through the premium experience and conditioning phases as evidenced by no measurable variation in the properties of visual dryness, trans-epidermal water loss, skin hydration, elastic extension, elastic recovery, firmness, total protein, the amount of one or more of Keratin 1, Keratin 10 and Keratin 11, and cytokine expression as compared with normal healthy control skin. It will be appreciated that the indicators of skin quality are not limited to those identified herein above and that other identifiers or indicators known in the art may also be assessed to determine improvement of skin quality according to the methods hereof.

Use of Biomarkers

One or more potential formulations of personal care compositions may screened against one or more biomarkers to assess efficacy of the composition with respect to skin improving benefit. Graphical data shown in the appendix of figures herein provides evidence regarding the results using the methods and compositions described herein.

Also provided are methods for improving the quality of skin that are evidenced by measurable improvement in one or more biomarker indicators. According to such methods, in some embodiments the steps include dispensing from a personal care article a personal care composition that comprises a hydrophobic benefit agent, applying the personal care composition to a user's skin together with water, rinsing the personal care composition from the user's skin, wherein a portion of the hydrophobic benefit agent is deposited and remains on the user's skin after rinsing. According to such embodiments, the steps further include repeating the steps of applying and rinsing on at least a once daily basis over a time interval of successive days, the time interval of use sufficient to permit detection of measurable improvement in at least one skin property selected from (i) reduction of visual dryness, a reduction in trans-epidermal water loss, increased skin hydration, increased elastic extension, increased elastic recovery, increased firmness and (ii) reduction in total protein, an increase in the amount of one or more of Keratin 1, Keratin 10 and Keratin 11, and a decrease in cytokine expression. In some such embodiments, the composition comprises a lathering agent and wherein the article operates to dispense the composition in aliquots, and wherein the ratio of lathering agent to hydrophobic benefit agent varies in successively dispensed aliquots of the composition over the course of dispensing the article contents such that the amount of hydrophobic benefit agent in two or more successive aliquots is different.

According to the various embodiments, evidence of improvement using biomarkers is determined using methods known in the art. For example, one or more such measurable improvement can include a reduction of visual dryness, a reduction in trans-epidermal water loss, increased skin hydration, wherein visual dryness is measured using corneometer and other known devices and techniques. In another example a measurable improvement is one or more of increased elastic extension, increased elastic recovery, increased firmness, measured using a cutometer and other known devices and techniques. In another example a measurable improvement is one or more of reduction in total protein, increase in the amount of one or more of Keratin 1, Keratin 10 and Keratin 11, decrease in one or more inflammatory cytokine expression, as measured from tissue or cell samples that may be obtained using known techniques such as skin strip methods described herein, biopsy, or other method of sampling. Measurements of total protein, specific proteins may be made using conventional techniques, and may include one or more affinity agents and assays as described herein and otherwise known in the art.

Also provided are methods for identifying a formulation comprising a hydrophobic benefit agent useful for improving the skin (stratum corneum barrier) in a human subject. Embodiments of such methods include generating one or more negative skin profiles for a human subject having dry or damaged skin; contacting the skin of the human subject with a proposed rinse-off personal care formulation by generating one or more test profiles and comparing the one or more test profiles to the one or more negative profiles and identifying the proposed formulation as effective if the test profile is directionally shifted away from the negative reference profile and shows at least one skin property selected from (i) reduction of visual dryness, a reduction in trans-epidermal water loss, increased skin hydration, increased elastic extension, increased elastic recovery, increased firmness and (ii) reduction in total protein, an increase in the amount of one or more of Keratin 1, Keratin 10 and Keratin 11, and a decrease in cytokine expression.

In one embodiment, the screening step comprises: (1) placing potential formulations of personal care composition in contact with skin or skin cells that exhibit need for improvement in terms of exhibiting any one or more signs of dryness or aging, the contact for a period of time sufficient to enable action on the skin tissue or cell. Typically, the time of action will be commensurate with the typical time of application of a rinse-off product as used conventionally; (2) repeating the treatment in parallel with control cells or tissue; (3) repeating the treatment in parallel with one or more control compositions, including, for example, water; (4) isolating samples from the skin or cells for analysis; (5) performing proteomic analysis and/or transcriptomic analysis and/or genomic analysis, partial or complete, for assessing the effect of the test composition; and (6) comparing the results with the controls.

Optimizing Compositions and Methods for Populations

It will be appreciated that the methods hereof are useful for benefiting users from a variety of populations. Accordingly, also provided are methods for developing personal care compositions and regimens of treatment for members of various populations. The methods involve understanding the preferences of the target populations. For example, North American consumers are accustomed to thicker personal care compositions and heavier skin feel than consumers in China. Accordingly, when designing a premium anti-aging body wash and methods of use, the personal care compositions must comply with regional expectations balanced with delivery of the consumer desired skin benefits. Thus, for example, for one target population, the personal care composition lipid profile varies from 25% to 55%, giving consumers not only improved personal care composition aesthetics and in-use experience, but optimal performance in terms of conditioning. For another target population, personal care composition lipid profile varies from 10-15% lipid. Similar preferences exist with respect to personal care composition texture, consistency, lather character and primary benefit focus. For example, while some eastern consumers expect personal care compositions that are of thinner consistency and lighter skin feel, other consumers are more similar to American consumers—expecting more from their personal care compositions, enjoying thicker consistencies and are more open to heavier skin feels. Thus, methods are provided for providing a range of personal care compositions (a global menu) for the consumers in various populations, such as populations that are defined geographically.

The various embodiments include identifying a target population and developing a population profile with respect to a rinse-off personal care composition used for cleansing and moisturizing comprising the steps of determining the population preferences for maximum amount of hydrophobic benefit agent, and determining the population preferences for lather volume, lather texture, and lathering speed, composition thickness, color, translucence, opalescence, and scent. Such embodiments further include the steps of formulating a personal care composition reflecting a population profile, wherein the composition comprises varying ratios of a lathering agent to a hydrophobic benefit agent, configuring a delivery article adapted to dispense the composition in discrete aliquots of approximately equal volume, and adapted to contain the composition so as to dispense the composition in phases comprising at least a first phase comprising a first ratio of the varying ratios of lathering agent to hydrophobic benefit agent, and a second phase comprising a second ratio of the varying ratios of lathering agent to hydrophobic benefit agent that is different than the first ratio. In some such embodiments, the steps further include manufacturing the composition for the target population; and providing the composition in the delivery article. It will be appreciated that the method may be repeated for a different target population.

III. Treatment Examples Example 1 Personal Care Composition Features and Benefits

Factors Benefits 1. Skin Enhancement Minimizing lines Improving skin tone Helping skin look younger 2. Rinsing/Clean Feel Not leaving skin greasy or coated Rinsing easily from skin Leaving skin feeling clean 3. Moisturization Not leaving skin dry/cracked Leaving skin soft/smooth Hydrating and locking in Moisture 4. Scent Having a pleasant scent during use Having a pleasant scent in bottle Leave long lasting scent on skin 5. Lather Providing right lather amount Lathering quickly and easily Providing rich, creamy lather

Example 2 Clinical Study: Evaluation of Skin Indicator Response

A study was undertaken to evaluate the response of a variety of skin indicators using an array of different personal care compositions and water. The study was 29 days in duration, with a 7 day interval of preconditioning, 21 days of treatment and 1 regression day. Skin was analyzed at various points from the beginning through the end of the study period. The objective of the study was to characterize the dry skin improvement profile of several body wash prototypes and to generate samples to assess treatment's effects on stratum corneum indicators (also referred to as biomarkers).

Leg wash studies are used to evaluate the beneficial effects of personal care products on dry leg skin. Leg wash studies are designed to approximate consumer-relevant exposure levels, e.g. washing frequency. The technique used in this study is a modification of a published procedure (Ertel, et al, 1999).

The study was conducted over 29 consecutive days, including a 7-day preconditioning phase, a 21-day treatment phase and 1 day of regression. This randomized study employed an incomplete block design in which 4 of the 5 treatments was evaluated on each subject, 2 treatments on each leg.

After the 7-day preconditioning phase, subjects returned to the test facility to have the skin on their lower legs evaluated by an expert grader. Only subjects which exhibited sufficient dryness on all of the treatment sites qualified to continue into the treatment phase.

Technicians treated each qualified subjects' lower legs in a controlled manner with the assigned treatments once daily for 21 days. Subjects' legs were visually evaluated for dryness and redness at several pre and post-treatment times as outlined in the following study schedule. Non-invasive instrumental measurements of stratum corneum hydration (Corneometer 825), barrier function (Dermalab TEWL (trans epidermal water loss)), and viscoelasticity (Cutometer) were made on the treatment sites following visual evaluations.

Preconditioning Phase Procedure

Prospective subjects were selected on the basis of their ability to meet the inclusion and exclusion criteria on DCF 1 and must have provided written informed consent. During preconditioning, enrolled subjects used a bar of Olay® with no exfoliating beads provided by the test facility in place of their usual product(s) for bathing and showering. They continued to use this product throughout their participation. Subjects also received a set of instructions to be followed during the study.

Treatment Phase Procedure

Before initial grading on Study Day 8, test facility personnel marked off the leg application areas [two 70 cm² areas (7 cm across×10 cm down)] on the outer aspect of the subjects' lower legs using a template and laboratory marking pen (corner brackets are sufficient to delineate each area). Trained clinical assistants treated each subject's legs according to the procedure outlined in the Treatment Procedure. In general, the following should be noted:

The “No Treatment” site (code A) was wetted initially, rinsed, and dried per the normal wash procedure. During the “product application” portion of the procedure, the site was timed for the 90 sec. “residence” but did not have product or additional water applied, nor underwent any of the physical manipulation (i.e., rubbing with fingers or implement).

Clinical Assistants wore disposable gloves during wash procedure, changed them between treatments and between subjects.

Clinical Assistants verified the correct treatment sequence and documented such before treating each subject.

The procedure was conducted once each day for 21 consecutive days.

The body wash products were applied using puffs. Puffs were pre-labeled with subject number and treatment code, and used accordingly throughout the treatment phase.

The puff treatment procedure for all puffs was conducted daily after all product treatments were completed on each subject (except on the final day of treatment).

Product/Puff Preparation and Placement

The Sponsor provided puffs for use in application of body washes. All of the puffs were treated with 9.3 ml of the appropriate treatment code each day after treatment (except on the final day of treatment.) according to the procedure outlined in the Treatment/Puff Treatment Procedure. All body wash products were dispensed at 0.7 ml (dose targeted at 10 μl/cm²). Products were mixed according to the procedures outlined in the Test Product Mixing Procedure. Briefly Code C was prepared by weighing out 10 g of product from individual bottles and then mixed. A sample of unused Code C was transferred to a jar, sealed, and sent to the Sponsor weekly for analysis. Two of the body wash products (codes B & E) were swirled dual component products that are supplied in a single container. A sufficient amount of each swirled product for all subjects for one day was dispensed into a dosing container and then stirred with a spatula until the product is well mixed. The mixed product was drawn into syringes at the 0.7 ml dosage.

Evaluations

At each evaluation, subjects acclimated for a minimum of 30 minutes in a room with the environment maintained at 70° F.±2 and 30-45% relative humidity prior to visual grading and non-invasive instrumental measurements being made on their legs.

All evaluations were made in the controlled environment described above. Instrumental measurements were made according to procedures outlined in the Sponsor's instructions or published guidelines. The same instruments and operators were used throughout the study.

Visual Grading

Each subject's lower legs were visually evaluated by a qualified grader for dryness and redness at baseline (Study Day 8, prior to the first treatment) as a prerequisite for qualification into the treatment phase.

The same grader was used throughout the study. Qualifying subjects were graded at the following 9 additional times during the course of the study:

Study Day 8—Baseline and approximately 3 hours post treatment #1;

Study Day 10—approximately 3 hours post treatment #3;

Study Days 12 & 21—approximately 24 hours post treatments #4 and #13 and approximately 3 hours post treatments #5 and #14;

Study Day 28—approximately 3 hours post treatment #21;

Study Day 29—approximately 24 hours post treatment #21;

Corneometer Skin Capacitance

Non-invasive skin capacitance measurements were taken in duplicate on each site of the subjects' legs after every visual grading during the study using a Corneometer CM825 instrument. Data was recorded electronically using the Sponsor's direct data entry and data capture programs. The same instrument and operator were used throughout the study

Trans-Epidermal Water Loss (TEWL)

TEWL was measured with the DermaLab® Evaporimeter equipped with dual probes. Each measurement consists of readings collected for 60 seconds with the mean of the last 20 seconds recorded from both probes (Channel A and Channel B). One measurement was taken at each treatment site and recorded on DCF 2 (DermaLab TEWL Measurements Log) on each evaluation day for both probes as Channel A and Channel B, respectively. The same instrument and operator were used throughout the study. These measurements were made according to procedures outlined in the Sponsor's instrument SOP or published guidelines. Measurements were taken 8 times during the course of the study;

Study Day 8—Baseline;

Study Day 10—approximately 3 hours post treatment #3;

Study Day 12—approximately 24 hours post treatment #4 and approximately 3 hours post treatment #5;

Study Day 21—approximately 24 hours post treatment #13 and approximately 3 hours post treatment #14;

Study Day 28—approximately 3 hours post treatment #21;

Study Day 29—approximately 24 hours post treatment #21.

Cutometer Measurements of Elasticity

Non-invasive skin viscoelasticity measurements were taken with a Cutometer SEM 575 equipped with an 8 mm probe. Data was recorded electronically using the data capture program accompanying the instrument. Two Cutometer instruments were used due to the number of subjects enrolled in the study. Subjects were assigned to the same instrument throughout the study on the basis of there subject number. The same instruments and operators were used throughout the study. These measurements were made according to the procedures outlined in the Sponsor's instrument SOPs or published guidelines. Measurements were taken 5 times during the course of the study;

Study Day 8—Baseline;

Study Day 10—approximately 1 hour post treatment #3;

Study Day 12—approximately 1 hour post treatment #5;

Study Day 21—approximately 1 hour post treatment #14;

Study Day 28—approximately 1 hour post treatment #21;

Imaging

Digital images were taken of full length, lower legs. Both left and right outer calves were taken for each subject. Images were captured with under both parallel and cross polarized lighting.

The leg imaging system (LIS) uses a combination of two cameras to capture both study images and repositioning images. Study images are captured with a Fuji F2 Pro digital SLR camera with a 60 mm Nikor lens. Repositioning images are captured with a SuperCircuits PC-33C CCD video camera with a Computar 8.5-40 mm f1.3 CS-mount lens. Using proprietary imaging software (UltraGrab), both the study and repositioning digital images are captured and stored on a portable personal computer while simultaneously being backed-up to an external USB hard drive or another networked workstation designated for backup file storage. Image illumination is provided by 1 JTL Versalight D 1000 flash unit with a color temperature around 5600 K provides the illumination for the study images. The camera and flash unit are mounted onto the imaging platform of the LIS, which also incorporates a fixed color chart used for the “on-the-fly” color calibration and color correction of study images. A changeable filter holder system is attached in front of the imaging camera which allows for the selection of the correct combination of filter alignment to capture both parallel and cross polarized images.

To capture an image each subject sat at the end of the imaging system with the leg positioning frame. Two leg rests are positioned (one each near the ankle and knee) such that the subject can easily place either of their outer legs (left or right) against each rest allowing the leg to be positioned such that it was in the center of the imaging area. The system was placed in a dedicated room at least 8×8 square feet or a curtained off area of a larger room. One electric circuit and wall outlet provided power to the image capturing system using one outlet power strip and a UPS power backup system. Measurements were taken 6 times during the course of the study;

Study Day 8—Baseline;

Study Day 10—approximately 3 hours post treatment #3;

Study Day 12—approximately 3 hours post treatment #5;

Study Day 21—approximately 3 hours post treatment #14;

Study Day 28—approximately 3 hours post treatment #21;

Study Day 29—approximately 24 hours post treatment #21

Tape Stripping

Tape stripping was performed throughout the study for dry skin sampling. D-Squames was always collected following all other evaluations scheduled to take place at the same time point. Clinical assistants wore disposable gloves while collecting D-Squames. At each collection time point a series of 6 D-Squames were used to sample the same spot within the treatment area. The technician used forceps to place a D-Squames sampling disc toward the edges of each site (away from the region being evaluated by other instrumentation) and applied pressure using the D-Squames disc applicator (push the D-Squames applicator down and then release). The technician removed the sampling disc with forceps and placed the disc into a pre-labeled 12 well culture plate. Each subject had two 12 well culture plates for sampling disc collection; one for each leg. Wells 1-6 of each plate were for the site nearest the knee, while wells 7-12 were used for the site nearest the ankle. D-Squames sample plates were placed in shipping boxes with labels corresponding to the subjects' samples enclosed and placed in a cooler with dry ice. The samples were couriered to the Sponsor's designee once all samples for the day have been collected. D-Squames was collected 4 times at the following time points:

Study Day 8—Baseline;

Study Day 12—approximately 24 hours post treatment #4;

Study Day 21—approximately 24 hours post treatment #13;

Study Day 29—approximately 24 hours post treatment #21;

References: Ertel, K. D., Neumann, P. B., Hartwig, P. M., Rains, G. Y., and Keswick, B. H., Leg Wash protocol to assess the skin moisturization potential of personal cleansing products. Int. J. Cosmet. Sci. 21: 383-397 (1999); Fitzpatrick, T. B., The validity and practicality of sun-reactive skin types I through VI. Arch. Dermatology, 124: 869-871 (1988).

Cytokine, Keratin and Soluble Protein Analyses

Samples were collected for analysis using D-Squame Tape Strips. D-Squame tapes were applied on the site of interest (Scalp, Leg, Face, Underarm, Forearm) with constant pressure/time, and removed to collect samples of the stratum corneum. Alternative sampling methods using Sebutape and Cup Scrubs can also be accommodated. Tape strip samples were placed in a 12 well plate under frozen conditions (−80° C.) until analysis. Tape samples were extracted for analysis by placing the tapes inside a polypropylene tube (2 ml) and adding extraction buffer (PBS, pH 7.4, 0.04% SDS, Protease Inhibitors) and sonicating for 30 min at 4° C. The samples were then centrifuged to remove any insoluble material and the supernatant is transferred into two deep well plates.

Supernatant samples for Cytokine/keratin analysis were fortified with 2.0% Bovine Serum Albumin (BSA) before freezing. The remaining supernatants were transferred to a second deep well plate for Soluble Protein analysis. Samples were analyzed for Cytokines (IL-1^(α), IL-1ra, IL-8) and Skin analytes (Human Serum Albumin, Keratin 1, 10, 11) using validated Millipore™ Multiplex immunoassay methods with a Bio-Plex Protein Array Reader system. Soluble protein determinations of the supernatants were performed using the Pierce BCA™ Protein assay kit with the aliquot designated for soluble protein using a validated method. The values obtained for soluble proteins were used to normalize the Cytokine and Keratin data. Cytokine and Skin analyte concentrations were reported as pg/mL or ng/mL and the soluble proteins were reported as μg/mL. Methods have been validated to demonstrate accuracy, precision, bench top stability, freeze thaw stability, short and long term storage stability of the extracts. Extraction efficiency of the methods have been shown to be >70% and reproducible with a single extraction of the tape strips.

Expected Biomarker Outcome for Endpoints Biomarkers Rationale Benefit Benefit Stratum Corneum Total Protein More cohesiveness ↓ Strengthening Cohesiveness in healthy stratum strateum corneum corneum. Less Improving skin cohesiveness in barrier. damaged skin. Differentiation Keratin 1, 10 Higher ↑ Improving skin 11 differentiation in health normal/healthy skin. Irritation/ Cytokines Elevated in ↓ Reducing skin Inflammation IL-1^(α), IL-1ra, diseased/irritated irritation. IL-8 skin.

Keratin 1, 10, 11 Results: The results of Keratin 1, 10, 11 were normalized to total soluble protein. The results are plotted below. A significant increase of normalized Keratin 1, 10 11 as compared to water control at day 7 (100% increase) was observed. The normalized Keratin 1, 10, 11 level is further increased to 150% vs. water at day 14 and 22. The data is consistent with literature reports that dry skin dry skin is a condition characterized by hyperproliferation and decreased differentiation. (See Engeke, Jensen, Ekanayake-Mudiyanselage and Proksch “Effects of xerosis and aging on epidermal proliferation and differentiation”, Br. J. Dermatology, 137: 219-225 (1997).)

Total Protein Results: The results of the total protein from six consecutive tape strips as measured by SquameScan 850 were obtained. Treatment according to the variable lipid method showed improved cohesiveness at day 7.0, 14.0, and 22.0 measurement points vs. water control.

Example 3 Improvements in Skin Elasticity and Cohesion from a Petrolatum Depositing Bodywash

Aging skin is frequently characterized by an increase in dryness and subsequent flaking, as well as a general loss of elasticity. Daily activities such as bathing can exacerbate some of these issues, particularly if skin drying products such as soap are used. While moisturizing bodywashes are readily available in the market, few purport to make improvements in skin condition beyond skin dryness.

Objective

In an effort to improve the overall condition, health and viability of aging skin, we have developed a petrolatum depositing bodywash that is aesthetically pleasing to use and will deliver benefits beyond typical moisturization.

Method

Standard Leg Controlled-Application Test (LCAT) methodology was used. Treatment was conducted over a 3 week period; women with dry leg skin had their legs washed once daily with the randomly assigned body wash products and water alone treatment as control (˜50 per treatment). Typical moisturization measures were taken, including expert dryness grading, corneometer and TEWL.

Non-invasive skin viscoelasticity measurements were taken with a Cutometer SEM 575. Tape-strip analysis of biomarkers was also conducted to gain insight into how the product affected the skin health and integrity. Six successive D-squame tapes were taken from virgin areas within each treatment site at baseline and at the end of each treatment week. The strips were then analyzed for total protein with a SquameScan 850 as a measure of stratum corneum cohesiveness. The method is based on a well established D-Squame tape strip procedure. Tape strip samples are subsequently extracted in appropriate buffer solution by sonication followed by centrifugation. The resulting supernatant samples are analyzed for relevant skin biomarkers (total proteins, cytokines, and keratin) by validated analytical methods (Multiplex ELISA and LC/MS/MS).

Results

Results indicate that the body wash delivers significant improvements in all standard moisturization measures (dryness grades, corneometer hydration, and TEWL). For the first time in the rinse-off context, the results show significant improvement in skin elasticity as compared to the water treatment control. The total protein results further reveal significant improvement in stratum corneum cohesiveness. Taken together, these findings support the conclusion that the petrolatum depositing bodywash improves the overall condition of skin.

Example 4 Test of Inventive Composition Example A

The following test of Inventive Composition Example A further demonstrates the benefits of articles, methods, and/or compositions used in accordance with the present invention.

Step A) Preconditioning Phase Procedure

-   -   During preconditioning, enrolled subjects used a bar of Olay®         with no exfoliating beads provided by the test facility in place         of their usual product(s) for bathing and showering. They         continued to use this product throughout their participation.

Step B). Treatment Phase Procedure

-   -   Before initial grading on Study Day 8, test facility personnel         marked off the leg application areas [two 70 cm² areas (7 cm         across×10 cm down)] on the outer aspect of the subjects' lower         legs using a template and laboratory marking pen (corner         brackets are sufficient to delineate each area). Trained         clinical assistants treated each subject's legs according to the         procedure outlined in the Treatment Procedure. In general, the         following should be noted:

Treatment Procedure:

-   -   Begin with the LEFT leg:     -   1. A Clinical Assistant wets the treatment area for 5 seconds         with 95-100° F. running tap water.     -   2. The Clinical Assistant applies the test product assigned to         that site, using the appropriate procedure as follows:     -   “No Treatment” (water only):         -   No product is applied to this site. Wait approximately 10             seconds, then continue as below with Step #3.         -   [The “No Treatment” site is wetted initially (#1), rinsed             (#5), and dried (#6) per the normal wash procedure. The site             is timed for the 90 sec. “residence” (#3) but does not have             product applied nor undergo any of the physical manipulation             (i.e., rubbing with fingers or implement).]     -   Body Wash Products:         -   While holding the appropriately labeled puff in one hand,             wet the puff for 5 seconds under the running tap, then allow             the excess water to drain off the puff for 10 seconds             without shaking or squeezing the puff.         -   Dispense 0.7 ml of body wash product from the syringe onto             the center of the treatment area.         -   Place the wet puff over the dispensed product and gently rub             the puff back and forth within the appropriate site for 10             seconds.     -   3. The lather (or water only) remains on the application site         for 90 seconds.     -   4. When the residence time for a particular application site has         expired, the Clinical Assistant will rinse the site for 15         seconds under a running tap, taking care not to rinse the         adjacent sites.     -   5. After the application area has been rinsed, the Clinical         Assistant gently pats the area dry with a disposable paper         towel.     -   6. Using the appropriate treatments, this entire procedure         (#1-5) is repeated on the lower site on the left leg before         conducting the entire procedure (#1-5) on the right leg.     -   Puff Treatment Procedure     -   1. While holding the appropriately labeled puff in one hand, wet         the puff for 5 seconds under the running tap, then allow the         excess water to drain off the puff for 10 seconds without         shaking or squeezing the puff.     -   2. Dispense 9.3 ml of appropriate body wash product onto the         puff in a broad circular pattern.     -   3. Hold puff in one hand. Squeeze puff until you just feel the         core. Do 10 rotations forward alternating hands, then repeat in         the opposite direction for 10 rotations alternating hands, for a         total of 20 rotations     -   4. Following the wash, while holding the puff in one hand, rinse         the puff for 20 seconds under the running tap, then allow the         excess water to drain off then hang to dry.

Step C). Evaluations

-   -   At each evaluation, subjects were acclimated for a minimum of 30         minutes in a room with the environment maintained at 70° F.±2         and 30-45% relative humidity prior to visual grading and         non-invasive instrumental measurements being made on their legs.         All evaluations were made in the controlled environment         described above.     -   1. Visual Grading:     -   Each subject's lower legs were visually evaluated by a qualified         grader for dryness at baseline (Study Day 8, prior to the first         treatment) as a prerequisite for qualification into the         treatment phase. The minimum entrance criteria are >2.5 in         initial dryness at the start of the treatment phase (Step B).     -   2. Cutometer Measurement of Skin Elasticity     -   The first cutometer measurement was performed before the initial         product treatment phase as baseline. The second set of cutometer         measurement was made at 90 mins after the seventh product         treatment. All non-invasive skin viscoelasticity measurements         were taken with a Cutometer® SEM 575 (Courage & Khazaka,         Electronic GmbH, Koeln, Germany) equipped with an 8 mm probe at         200 mbar pressure. The same instruments and operators were used         throughout the study. The following elastic parameters are         typically used: elastic extension U_(e), elastic recovery U_(r),         and elasticity R₇.     -   The cutometer's operating principles and applications are         described in reference below: A. O, Barel, W. Courage, P.         Clarys; Suction Method for Measurement of Skin Mechanical         Properties, the Cutometer®; Handbook of Non-Invasive Methods and         the Skin, J. Serup G. B. E. Jemec, 1995; 335-340.     -   3. Tape Stripping Procedure and Total Stratum Corneum Protein         Measurement     -   A first set of tape stripping was performed before the initial         product treatment phase as baseline. The second set of tape         stripping was performed at 24 hours after the sixth product         treatment. Clinical assistants wore disposable gloves while         collecting D-Squames®. At each collection time point a series of         6 D-Squames were used to sample the same spot within the         treatment area. The technician used forceps to place a D-Squame®         sampling disc toward the edges of each site (away from the         region being evaluated by other instrumentation) and apply         pressure using the D-Squame disc applicator (push the D-Squame         applicator down and then release). The technician then removed         the sampling disc with forceps and placed the disc into a         pre-labeled 12 well culture plate. Each subject had two 12 well         culture plates for sampling disc collection; one for each leg.     -   The total stratum corneum proteins are analyzed by infrared         densitometry (model number SquameScan® 850A, Heiland Electronic,         Wetzlar, Germany). The results are reported as protein         absorptance at 850 nm. The method is described in reference: R.         Voegeli, J. Heiland, S. Doppler, A. V. Rawlings and T. Schreier;         Efficient and simple quantification of stratum corneum proteins         on tape strippings by infrared densitometry, Skin Research and         Technology 2007; 13; 242-251.

Step D). Calculation of Skin Elasticity Improvement Index and Stratum Corneum Cohesiveness Improvement Index

-   -   1) Calculation of Skin Elasticity Improvement Index         -   a) Elastic Extension (U_(e)) Improvement Index is calculated             as:

[(U_(e))^(P) _(end)−(U_(e))^(C) _(end)]/(U_(e))^(C) _(end)*100−[(U_(e))^(P) _(ini)−(U_(e))^(C) _(ini)]/(U_(e))^(C) _(ini)*100

-   -   -   wherein             -   (U_(e))^(C) _(ini) is the initial elastic extension                 parameter at the beginning of the water control leg;             -   (U_(e))^(P) _(ini) is the initial elastic extension                 parameter at the beginning of the test product leg;             -   (U_(e))^(C) _(end) is the final elastic extension                 parameter at the end of the water control leg;             -   (U_(e))^(P) _(end) is the final elastic extension                 parameter at the end of the test product leg.         -   b) Elastic Recovery (U_(r)) Improvement Index is calculated             as:

[(U_(r))^(P) _(end)−(U_(r))^(C) _(end)]/(U_(r))^(C) _(end)*100−[(U_(r))^(P) _(ini)−(U_(r))^(C) _(ini)]/(U_(r))^(C) _(ini)*100 wherein

-   -   -   -   (U_(r))^(C) _(ini) is the initial elastic recovery                 parameter at the beginning of the water control leg;             -   (U_(r))^(P) _(ini) is the initial elastic recovery at                 the beginning of the test product leg;             -   (U_(r))^(C) _(end) is the final elastic recovery at the                 end of the water control leg;             -   (U_(r))^(P) _(end) is the final elastic recovery at the                 end of the test product leg.

        -   c) Elasticity (R₇) Improvement Index is calculated as:

[(R₇)^(P) _(end)−(R₇)^(C) _(end)]/(R₇)^(C) _(end)*100−[(R₇)^(P) _(ini)−(R₇)^(C) _(ini)]/(R₇)^(C) _(ini)*100

-   -   -   wherein             -   (R₇)^(C) _(ini) is the initial elasticity at the                 beginning of the water control leg;             -   (R₇)^(P) _(ini) is the initial elasticity at the                 beginning of the test product leg;             -   (R_(7r))^(C) _(end) is the final elasticity at the end                 of the water control leg;             -   (R₇)^(P) _(end) is the final elasticity at the end of                 the test product leg.

2) Calculation of Stratum Corneum Cohesiveness Improvement Index

-   -   a) Stratum Corneum Cohesiveness Improvement Index is calculated         as:

[(Protein)^(C) _(end)−(Protein)^(P) _(end)]/(Protein)^(C) _(end)*100−[(Protein)^(C) _(ini)−(Protein)^(P) _(ini)]/(Protein)^(C) _(ini)*100 wherein

-   -   (Protein)^(C) _(ini) is the sum of initial protein absorption of         tape 1 to tape 6 at the beginning of the water control leg;     -   (Protein _(e))^(P) _(ini) is the sum of initial protein         absorption of tape 1 to tape 6 at the beginning of the test         product leg;     -   (Protein)^(C) _(end) the sum of final protein absorption of tape         1 to tape 6 at the end of the water control leg;     -   (Protein)^(P) _(end) is the sum of final protein absorption of         tape 1 to tape 6 at the end of the test product leg.

3) Calculation of Keratin 1, 10, 11 Improvement Index

-   -   Keratin 1, 10, 11 Improvement Index is calculated as:

[(Keratin)^(C) _(end)−(Keratin)^(P) _(end)]/(Keratin)^(C) _(end)*100−[(Keratin)^(C) _(ini)−(Keratin)^(P) _(ini)]/(Keratin)^(C) _(ini)*100 wherein

-   -   (Keratin)^(C) _(ini) is the initial Keratin 1, 10, 11 normalized         to total soluble protein at the beginning of the water control         leg;     -   (Keratin)^(P) _(ini) is the initial Keratin 1, 10, 11 normalized         to total soluble protein at the beginning of the test product         leg;     -   (Keratin)^(C) _(end) is the final Keratin 1, 10, 11 normalized         to total soluble protein at the end of the water control leg;     -   (Keratin)^(P) _(end) is the final Keratin 1, 10, 11 normalized         to total soluble protein at end of the test product leg.         Results of Inventive Composition Example A vs. Water Control

Inventive p value Example A (base size n = 50) a) Skin Elastic Extension (Ue) 16 p = 0.003 Improvement Index b) Skin Elastic Recovery (Ur) 21 p = 0.0004 Improvement Index c) Skin Elasticity (R7) Improvement 4 p = 0.05 Index d) Stratum Corneum Cohesiveness 23 p < 0.0001 Improvement Index e) Keratin Improvement Index 172 p < 0.0001

IV. Personal Care Articles and Personal Care Compositions

The present invention contemplates use of personal care compositions and articles comprising personal care compositions. In some embodiments, personal care articles for dispensing a personal care compositions comprises a single chamber package and a personal care article. It will be appreciated that other embodiments of personal care articles and personal care compositions are contemplated for use according to the invention, and the following descriptions regarding possible embodiments is non-limiting.

Single chamber package comprises a dispensing orifice, a first zone proximal to the dispensing orifice, a second zone medial to the dispensing orifice, and a third zone distal to the dispensing orifice. The personal care article comprises a first personal care composition, a second personal care composition and a third personal care composition. The first personal care composition is substantially within the first zone and comprises a first concentration of a hydrophobic benefit material. The second personal care composition is substantially within the second zone and comprises a second concentration of a hydrophobic benefit material. The third personal care composition is substantially within the third zone and comprises a third concentration of a hydrophobic benefit material. The second concentration is greater than the first concentration and the third concentration of the hydrophobic benefit material. The first personal care composition is capable of being substantially dispensed prior to the second personal care composition and the third personal care composition. The second personal care composition is capable of being substantially dispensed prior to the third personal care composition.

The personal care article used in accordance with the present invention, in most embodiments, is statically stable. In most embodiments, the personal care article used in accordance with the present invention is dynamically stable according to the Dynamic Stability Shipping Method disclosed in the Test Methods below.

In some embodiments, the first personal care composition is in physical contact with the second personal care composition within the single chamber package. The second personal care composition, in another embodiment, is in physical contact with the third personal care composition within the single chamber package.

In one embodiment, the first zone, second zone and/or third zone of the present invention comprises from about 10% to about 70%, by volume, of the package. The first zone, second zone and/or third zone of the present invention comprise from about 10% to about 60%, from about 10% to about 50%, from about 10% to about 40%, from about 10% to about 30%, from about 10% to about 20%, by volume, of the package. In other embodiments, the first zone, second zone and/or third zone of the present invention comprises from about 20% to about 70%, from about 20% to about 60%, from about 20% to about 50%, from about 20% to about 40%, from about 20% to about 30%, by volume, of the package. In other embodiments, the first second and/or third zone of the present invention comprises from about 30% to about 70%, from about 30% to about 60%, from about 30% to about 50%, from about 30% to about 40%, by volume, of the package.

The personal care article used in accordance with the present invention comprises a single chamber package can contain any number or zones and compositions, such as for example, four zones and four compositions, five zones and five compositions, six zones and six compositions, twelve zones and twelve compositions, and so on. Each of these compositions is capable of substantially dispensing prior to the composition before it in a substantially sequential manner. For example, the fourth personal care composition substantially within the fourth zone is capable of dispensing prior to the fifth personal care composition within the fifth zone, etc. In some embodiments, a dual-chamber delivery article having side-by-side chambers with a control valve or cap to regulate dispensing from each chamber may be used. In other embodiments, a dual-chamber delivery article with end-to-end chambers may be selected, where product is dispensed separately from each chamber. In yet other embodiments, a kit of two or more separate bottles that may nest or stack or otherwise inter-fit may be used for dispensing the personal care compositions.

The personal care article used in accordance with the present invention is filled to comprise a headspace. In some embodiments, the personal care article used in accordance with the present invention comprises a headspace that is less than 10%, is less than 6%, less than 5% and less than 4%. In other embodiments, the personal care article used in accordance with the present invention comprises a headspace that is less than 3%, less than 2% and less than 1%.

In another aspect, each personal care composition comprises a dye, colorant or the like, such that each personal care composition is a distinct color or hue. For example, the first personal care composition is a yellow color, the second personal care composition is an orange color and the third personal care composition is a purple color.

The amount or concentration of hydrophobic benefit materials in the first personal care composition, second personal care composition and third personal care composition are usually formulated, by weight of the composition, at less than about 75%, less than about 65%, less than about 60%, less than about 60%, less than about 55%, less than about 50%, less than about 45%, less than about 40%, less than about 35%, less than about 30%, less than about 25%, less than about 20%, less than about 10%, less than about 5%, less than about 4%, less than about 3%, less than about 2%, less than about 1%. The first personal care composition, second personal care composition and third personal care composition comprises from about 1.0% to about 60%, from about 5% to about 60%, from about 10% to about 50%, from about 20% to about 45%, by weight of the personal care composition, of a hydrophobic benefit material.

In some embodiments, the first concentration can comprise from about 10% to less than about 50% or, from about 10% to about 40%, by weight of the first personal care composition. The first concentration of hydrophobic material, in other embodiments, comprise from about 15% to less than 45% or 15% to less than 35% by weight of the first personal care composition, of hydrophobic benefit material. The first concentration, in some embodiments, comprise from about 20% to about 40% and from about 25% to about 40%, by weight of the first personal care composition.

In some embodiments, the second concentration comprises from greater than 30% to about 70%, greater than about 35% to about 65%, by weight of the second personal care composition, of hydrophobic benefit material. In another embodiment, the second concentration comprises from about 40 to about 60% and about 55% by weight of the second personal care composition.

In some embodiments, the third concentration can comprise from about 10% to less than about 50% or, from about 10% to about 40%, by weight of the third personal care composition. The third concentration of hydrophobic material, in other embodiments, comprise from about 15% to less than 45% or 15% to less than 35% by weight of the third personal care composition, of hydrophobic benefit material. The third concentration, in some embodiments, comprise from about 20% to about 40% and from about 25% to about 40%, by weight of the third personal care composition.

In one embodiment, the first personal care composition, second personal care composition and third personal care composition used in accordance with the present invention are multi-phase compositions and comprise one of more phases or one or more of the components described in the phases below:

The personal care compositions used in accordance with the present invention comprise a benefit phase or benefit phase components. The benefit phase in the present invention, in most embodiments, is anhydrous and is substantially free of water. In some embodiments, the benefit phase is substantially free or free of surfactant.

Hydrophobic benefit materials suitable for use in the present invention typically have a Vaughan Solubility Parameter of from about 5 (cal/cm³)^(1/2) to about 15 (cal/cm³)^(1/2), as defined by Vaughan in Cosmetics and Toiletries, Vol. 103. The Vaughan Solubility Parameter (VSP) as used herein is a parameter used to define the solubility of hydrophobic materials. Vaughan Solubility parameters are well known in the various chemical and formulation arts and typically have a range of from 5 to 25. Non-limiting examples of hydrophobic benefit materials having VSP values ranging from about 5 to about 15 include the following: Cyclomethicone 5.92, Squalene 6.03, Petrolatum 7.33, Isopropyl Palmitate 7.78, Isopropyl Myristate 8.02, Castor Oil 8.90, Cholesterol 9.55, as reported in Solubility, Effects in Product, Package, Penetration and Preservation, C. D. Vaughan, Cosmetics and Toiletries, Vol. 103, October 1988.

The hydrophobic benefit materials for use in the benefit phase of the composition have a preferred rheology profile as defined by Consistency value (k) and Shear Index (n). The term “Consistency value” or “k” as used herein is a measure of lipid viscosity and is used in combination with Shear Index, to define viscosity for materials whose viscosity is a function of shear. The measurements are made at 35° C. and the units are poise (equal to 100 cps). The term “Shear Index” or “n” as used herein is a measure of lipid viscosity and is used in combination with Consistency value, to define viscosity for materials whose viscosity is a function of shear. The measurements are made at 35° C. and the units are dimensionless. Consistency value (k) and Shear Index (n) are more fully described in the Test Methods below. Preferred Consistency value ranges are 1-10,000 poise (1/sec)^(n−1), typically 10-2000 poise (1/sec)^(n−1) and more typically 50-1000 poise (1/sec)^(n−1). Shear Index ranges are 0.1-0.8, typically 0.1-0.5 and more typically 0.20-0.4. These preferred rheological properties are especially useful in providing the personal cleansing compositions with improved deposition of benefit agents on skin.

In one embodiment, the benefit phase is comprised of the hydrophobic benefit materials selected from the group consisting of petrolatum, lanolin, derivatives of lanolin (e.g. lanolin oil, isopropyl lanolate, acetylated lanolin, acetylated lanolin alcohols, lanolin alcohol linoleate, lanolin alcohol riconoleate) hydrocarbon oils (e.g. mineral oil) natural and synthetic waxes (e.g. micro-crystalline waxes, paraffins, ozokerite, lanolin wax, lanolin alcohols, lanolin fatty acids, polyethylene, polybutene, polydecene, pentahydrosqualene) volatile or non-volatile organosiloxanes and their derivatives (e.g. dimethicones, cyclomethicones, alkyl siloxanes, polymethylsiloxanes, methylphenylpolysiloxanes), natural and synthetic triglycerides (e.g. castor oil, soy bean oil, sunflower seed oil, maleated soy bean oil, safflower oil, cotton seed oil, corn oil, walnut oil, peanut oil, olive oil, cod liver oil, almond oil, avocado oil, palm oil, sesame oil) and combinations thereof. In one aspect, at least about 50% by weight of the hydrophobic benefit materials are selected from the groups of petrolatum, mineral oil, paraffins, polyethylene, polybutene, polydecene, dimethicones, alkyl siloxanes, cyclomethicones, lanolin, lanolin oil, lanolin wax. In one embodiment, the remainder of the hydrophobic benefit material is selected from: isopropyl palmitate, cetyl riconoleate, octyl isononanoate, octyl palmitate, isocetyl stearate, hydroxylated milk glyceride and combinations thereof. The benefit phase of the personal care composition, in some embodiments, comprises a combination of petrolatum and mineral oil.

In some embodiments, the personal care composition used in accordance with the present invention comprises a surfactant phase. The personal care composition typically comprises from about 1% to about 100%, by weight of the composition; from about 5% to about 85%; by weight of the composition, from about 10% to 80%, by weight of the composition; from about 20 to 70%, by weight of the composition; from about 25% to 60%, by weight of the composition, from about 30% to about 50%, by weight of the composition, of a surfactant phase.

In some embodiments, the surfactant phase comprises a structured domain that is comprised of a mixture of surfactants. The presence of structured domain enables the incorporation of high levels of hydrophobic benefit materials in a separate phase which is not emulsified within composition. In one aspect, the structured domain in the composition is characterized as, or is, an opaque structured domain. In one aspect, the opaque structured domain is characterized as, or is, a lamellar phase. The lamellar phase produces a lamellar gel network. The lamellar phase provides resistance to shear, adequate yield to suspend particles and droplets and at the same time provides long term stability, since it is thermodynamically stable. The lamellar phase tends to have a higher viscosity thus minimizing the need for viscosity modifiers.

In one aspect, the surfactant phase comprises a domain that is comprised of a mixture of surfactants and is a micellar phase. A micellar phase is optically isotropic. Micelles are approximately spherical in shape. Other shapes such as ellipsoids, cylinders, and bilayers are also possible. In one aspect, the micellar phase is structured to enhance viscosity and to suspend particles. This can be accomplished using viscosity modifiers such as those defined below as water structurants.

In some embodiments, the surfactant phase comprises a surfactant component which comprises of a mixture of surfactants including lathering surfactants or a mixture of lathering surfactants. The surfactant phase comprises surfactants suitable for application to the mammalian skin or hair and is compatible with water and the other ingredients of the composition used in accordance with the present invention. These surfactants include anionic, nonionic, cationic, zwitterionic, amphoteric, soap, or combinations thereof. Typically, anionic surfactant comprises at least 40% of the surfactant component. The personal care composition, in some embodiments, comprises the surfactant component at concentrations ranging from about 2% to about 40%, from about 4% to about 25%, about 1% to about 21%, about 3 to 15%, by weight of the composition, of the surfactant component.

Suitable surfactants are described in McCutcheon's, Detergents and Emulsifiers, North American edition (1986), published by allured Publishing Corporation; and McCutcheon's, Functional Materials, North American Edition (1992); and in U.S. Pat. No. 3,929,678 issued to Laughlin, et al on Dec. 30, 1975.

Preferred linear anionic surfactants for use in the surfactant phase of the personal care composition include ammonium lauryl sulfate, ammonium laureth sulfate, sodium lauryl sulfate, sodium laureth sulfate, potassium laureth sulfate, sodium lauryl sarcosinate, sodium lauroyl sarcosinate, lauryl sarcosine, cocoyl sarcosine, ammonium cocoyl sulfate, potassium lauryl sulfate, and combinations thereof.

Branched anionic surfactants and monomethyl branched anionic surfactants suitable for the present invention are described in a commonly owned U.S. Publication No. 60/680,149 entitled “Structured Multi-phased Personal Cleansing Compositions Comprising Branched Anionic Surfactants” filed on May 12, 2005 by Smith, et al. Branched anionic surfactants include but are not limited to the following surfactants: sodium trideceth sulfate, sodium tridecyl sulfate, sodium C₁₂₋₁₃ alkyl sulfate, and C₁₂₋₁₃ pareth sulfate and sodium C₁₂₋₁₃ pareth-n sulfate.

In one aspect of the personal care compositions used in accordance with the present invention comprise an amphoteric surfactant, a zwitterionic surfactant and combinations thereof. In one embodiment, the personal care composition comprises at least one amphoteric surfactant. Amphoteric surfactant suitable for use in the present invention include those that are broadly described as derivatives of aliphatic secondary and tertiary amines in which the aliphatic radical can be straight or branched chain and wherein one of the aliphatic substituents contains from about 8 to about 18 carbon atoms and one contains an anionic water solubilizing group, e.g., carboxy, sulfonate, sulfate, phosphate, or phosphonate. Examples of compounds falling within this definition are sodium 3-dodecyl-aminopropionate, sodium 3-dodecylaminopropane sulfonate, sodium lauryl sarcosinate, N-alkyltaurines such as the one prepared by reacting dodecylamine with sodium isethionate according to the teaching of U.S. Pat. No. 2,658,072, N-higher alkyl aspartic acids such as those produced according to the teaching of U.S. Pat. No. 2,438,091, and the products described in U.S. Pat. No. 2,528,378. In one aspect, the personal care composition comprises an amphoteric surfactant that is selected from the group consisting of sodium lauroamphoacetate, sodium cocoamphoactetate, disodium lauroamphoacetate disodium cocodiamphoacetate, and combinations thereof. Moreover, Amphoacetates and diamphoacetates are also used in some embodiments of the present invention.

Zwitterionic surfactants suitable for use include those that are broadly described as derivatives of aliphatic quaternary ammonium, phosphonium, and sulfonium compounds, in which the aliphatic radicals can be straight or branched chain, and wherein one of the aliphatic substituents contains from about 8 to about 18 carbon atoms and one contains an anionic group, e.g., carboxy, sulfonate, sulfate, phosphate, or phosphonate. Zwitterionic surfactants suitable for use in the personal care composition include alkyl betaines, including cocoamidopropyl betaine.

The personal care composition used in accordance with the present invention is typically free of alkyl amines and alkanolamide to ensure mildness of the composition to the skin.

An electrolyte can be added per se to the personal care composition or it can be formed in situ via the counterions included in one of the raw materials. The electrolyte typically includes an anion comprising phosphate, chloride, sulfate or citrate and a cation comprising sodium, ammonium, potassium, magnesium or combinations thereof. Some preferred electrolytes are sodium chloride, ammonium chloride, sodium or ammonium sulfate. The electrolyte is typically added to the surfactant phase of the composition in the amount of from about 0.1% to about 6%; from about 1% to about 5%, more typically from about 2% to about 4%, more typically from about 3% to about 4%, by weight of the personal care composition.

In one embodiment, the first personal care composition comprise a first concentration of surfactant, the second personal care composition comprises a second concentration of surfactant and the third personal care composition comprises a third concentration of surfactant. The first concentration of surfactant is different from the second concentration of surfactant and the third concentration of surfactant, in some embodiments. In one aspect, the first personal care composition has a first concentration of surfactant that is a greater that the second concentration of surfactant in the second personal care compositions and is the same as or greater than the third concentration of surfactant in the third personal care compositions. In one aspect, the first personal care composition has a lower concentration of surfactant than the second and the third personal care compositions.

In some embodiments, the personal care compositions used in accordance with the present invention comprise a structured aqueous phase. The structured aqueous phase, in one embodiment, comprises a water structurant and water. The structured aqueous phase has a pH in the range from about 5 to about 9.5, or in one aspect have a pH of about 7. In one embodiment, the structured aqueous phase is hydrophilic. In one aspect, the structured aqueous phase is a hydrophilic, non-lathering gelled water phase.

In some embodiments, the structured aqueous phase comprises less than about 5%, less than about 3%, less than about 1%, by weight of the structured aqueous phase, of a surfactant component. In one aspect, the structured aqueous phase is free of lathering surfactants in the composition. In one embodiment, the structured aqueous phase of the present invention comprises from about 30% to about 99%, more than about 50%, more than about 60%, more than about 70%, more than about 80%, by weight of the structured aqueous phase, of water.

In one embodiment, the structured aqueous phase comprises a water structurant. The water structurant is selected from the group consisting of inorganic water structurants (e.g. silicas, polyacrylates, polyacrylamides, modified starches, crosslinked polymeric gellants, copolymers) charged polymeric water structurants (e.g. Acrylates/Vinyl Isodecanoate Crosspolymer available, STABYLEN 30® available from 3V SIGMA S.P.A of Bergamo Italy), Acrylates/C10-30 Alkyl Acrylate Crosspolymer (e.g. PEMULEN™ TR1 and TR2 polymers available from NOVEON®), Carbomers, Ammonium Acryloyldimethyltaurate/VP Copolymer (e.g. Aristoflex® AVC available from Clariant), Ammonium Acryloyldimethyltaurate/Beheneth-25 Methacrylate Crosspolymer (e.g. ARISTOFLEX® HMB available from Clariant), Acrylates/Ceteth-20 Itaconate Copolymer (e.g. STRUCTURE® 3001 available from National Starch), Polyacrylamide (e.g. SEPIGEL™ 305 available from SEPPIC), water soluble polymeric structurants (e.g. cellulose gums and gel, and starches), associative water structurants (e.g. xanthum gum, gellum gum, pectins, alginates such as propylene glycol alginate), and combinations thereof. In some embodiments, the structured aqueous phase comprises from about 0.1% to about 30%, from about 0.5% to about 20%, from about 0.5% to about 10%, and from about 0.5% to about 5%, by weight of the structured aqueous phase, of a water structurant. In some embodiments, a water structurant for the structured aqueous phase has a net cationic charge, net anionic charge, or neutral charge.

While not essential for the purposes of the present invention, the non-limiting list of optional materials, illustrated hereinafter are suitable for use in personal care compositions, and may be incorporated in certain embodiments, for example to assist or enhance cleansing performance, for treatment of the skin, or to modify the aesthetics of the personal care composition. Optional materials useful in the products herein are described by their cosmetic and/or therapeutic benefit or their postulated mode of action or function. These descriptions are non-limiting and made for the sake of convenience because it is understood that these materials can provide more than one benefit, function or operate via more than one mode of action. The precise nature of these optional materials, and levels of incorporation thereof, will depend on the physical form of the composition and the nature of the cleansing operation for which it is to be used. The amount of optional materials in compositions are usually formulated, by weight of the composition, at less than about less than about 6%, less than about 5%, less than about 4%, less than about 3%, less than about 2%, less than about 1%, less than about 0.5%, less than about 0.25%, less than about 0.1%, less than about 0.01%, less than about 0.005%.

In some embodiments of the present invention, comprise optional ingredients, which are selected from the group consisting of thickening agents, low density microspheres (e.g. EXPANCEL® microspheres available from 091 WE40 d24, Akzo Nobel and others described in commonly owned and assigned U.S. Patent Publication No. 2004/0092415A1 published on May 13, 2004), preservatives, antimicrobials, fragrances, chelators (e.g. such as those described in U.S. Pat. No. 5,487,884 issued to Bisset et al.), sequestrants, vitamins (e.g. Retinol), vitamin derivatives (e.g. tocophenyl actetate, niacinamide, panthenol), sunscreens, desquamation actives (e.g. such as those described in U.S. Pat. Nos. 5,681,852 and 5,652,228 issued to Bisset), anti-wrinkle/anti-atrophy actives (e.g. N-acetyl derivatives, thiols, hydroxyl acids, phenol), anti-oxidants (e.g. ascorbic acid derivatives, tocophenol), skin soothing agents/skin healing agents (e.g. panthenoic acid derivatives, aloe vera, allantoin), skin lightening agents (e.g. kojic acid, arbutin, ascorbic acid derivatives), skin tanning agents (e.g. dihydroxyacteone), polymeric phase structurant (e.g. naturally derived polymers, synthetic polymers, crosslinked polymers, block copolymers, copolymers, hydrophilic polymers, nonionic polymers, anionic polymers, hydrophobic polymers, hydrophobically modified polymers, associative polymers, and oligomers); a liquid crystalline phase inducing structurant (e.g. trihydroxystearin available from Rheox, Inc. under the trade name THIXCIN® R), organic cationic deposition polymer (e.g. Polyquaternium 10 available from Amerchol Corp., guar hydroxypropyltrimonium chloride available as JAGUAR® C-17 from Rhodia Inc., and N-HANCE® polymer series commercially available from AQUALON), pH regulators (e.g. triethanolamine), anti-acne medicaments, essential oils, sensates, pigments, colorants, pearlescent agents, interference pigments (e.g. such as those disclosed in U.S. Pat. No. 6,395,691 issued to Liang Sheng Tsaur, U.S. Pat. No. 6,645,511 issued to Aronson et al., U.S. Pat. No. 6,759,376 issued to Zhang et al., U.S. Pat. No. 6,780,826 issued to Zhang et al.) particles (e.g. talc, kolin, mica, smectite clay, cellulose powder, polysiloxane, silicas, carbonates, titanium dioxide, polyethylene beads) hydrophobically modified non-platelet particles (e.g. hydrophobically modified titanium dioxide and other materials described in a commonly owned, patent application published on Aug. 17, 2006 under Publication No. 2006/0182699A by Taylor, et al.) and combinations thereof. Other optional ingredients are most typically those materials approved for use in cosmetics and that are described in the CTFA Cosmetic Ingredient Handbook, Second Edition, The Cosmetic, Toiletries, and Fragrance Association, Inc. 1988, 1992.

V. Methods Related to Personal Care Articles and Personal Care Compositions Measuring Lather Volume

Lather volume of a personal skin care composition can be measured using a graduated cylinder and a tumbling apparatus. A 1,000 ml graduated cylinder is chosen which is marked in 10 ml increments and has a height of 14.5 inches at the 1,000 ml mark from the inside of its base (for example, Pyrex No. 2982). Distilled water (100 grams at 23° C.) is added to the graduated cylinder. The cylinder is clamped in a rotating device which clamps the cylinder with an axis of rotation that transects the center of the graduated cylinder. One gram of the total personal cleansing composition with specified cleansing phase to benefit phase ratio (0.75 g of the cleansing phase and 0.25 g of the benefit phase, or 0.45 g of the cleansing phase and 0.55 g of the benefit phase) is added into the graduated cylinder and the cylinder is capped. The cylinder is rotated at a rate of 10 revolutions in about 20 seconds, and stopped in a vertical position to complete the first rotation sequence. A timer is set to allow 30 seconds for the lather thus generated to drain. After 30 seconds of such drainage, the first lather volume is measured to the nearest 10 ml mark by recording the lather height in ml up from the base (including any water that has drained to the bottom on top of which the lather is floating).

If the top surface of the lather is uneven, the lowest height at which it is possible to see halfway across the graduated cylinder is the first lather volume (ml). If the lather is so coarse that a single or only a few foam cells (“bubbles”) reach across the entire cylinder, the height at which at least 10 foam cells are required to fill the space is the first lather volume, also in ml up from the base. Foam cells larger than one inch in any dimension, no matter where they occur, are designated as unfilled air instead of lather. Foam that collects on the top of the graduated cylinder but does not drain is also incorporated in the measurement if the foam on the top is in its own continuous layer, by adding the ml of foam collected there using a ruler to measure thickness of the layer, to the ml of foam measured up from the base. The maximum foam height is 1,000 ml (even if the total foam height exceeds the 1,000 ml mark on the graduated cylinder). One minute after the first rotation is completed, a second rotation sequence is commenced which is identical in speed and duration to the first rotation sequence. The second lather volume is recorded in the same manner as the first, after the same 30 seconds of drainage time. A third sequence is completed and the third lather volume is measured in the same manner, with the same pause between each for drainage and taking the measurement.

The lather result after each sequence is added together and the Total Lather Volume determined as the sum of the three measurements, in ml. The Flash Lather Volume is the result after the first rotation sequence only, in ml, i.e., the first lather volume. Compositions according to the present invention perform significantly better in this test than similar compositions in conventional emulsion form.

Microcentrifugation Method:

The Microcentrifugation Method determines the variation of the percent of hydrophobic benefit material per dose in a package that comprises a personal care article. As an overview, the personal care articles being tested are dispensed in 10.0 mL sample sizes and these samples are centrifuged. Centrifugation separates the sample size of personal care articles into distinguishable layers. The first personal care composition, second personal care composition and third personal care composition have multiple distinguishable layers, for example a microsphere layer, a surfactant layer, and a benefit layer that comprises hydrophobic benefit material, as shown in FIG. 2B and FIG. 2C. After centrifugation, the volume percentage of the benefit phase for each sample is determined and plotted per dose of personal care article to obtain the hydrophobic benefit material distribution profile of the personal care article throughout the product package.

TABLE 1 Description of Apparatus used in the Microcentrifugation Method Apparatus: Description: Micro-centrifuge VWR Galaxy 16DH 2 mL Micro-centrifuge VWR cat. No. 20170-170 clear tubes Disposable syringes 1 mL, VWR cat. No. BD309602 Top Load balance Capable of weighing to 2 decimal cases. Clear plastic cups 207 mL Solo Plastic cup Centrifuge tube stand capacity to hold at least 24 tubes Electronic Digital Caliper capable of measuring 2 decimal cases in mm

To prepare the samples for a 295 mL package of a personal care article, label 24 clear plastic cups 1-24. Place cup 1 on top of balance and tare. Open package containing the personal care article, dispense 8.80 g±0.50 g of product in cup 1, and record the weight of each sample. Repeat these instructions for all 24 cups, or for as many doses you can get from one package. If composition gets stuck in the package, tap the package in descending motion for four times.

Next, label 24 centrifuge tubes 1-24 doses. Then, mix the sample in cup 1 well by stirring the sample with a stirrer by hand and then draw the sample into a syringe. Insert the syringe all the way to the bottom of the centrifuge tube. Slowly push the plunger as you withdraw the syringe form the centrifuge tube, making sure no air bubbles or gaps are formed. Check for air bubbles, if any air bubble is found tap the centrifuge tube until sample fills the gaps left by the air bubbles. Load the syringe with more sample of the product and bring the extremity of the syringe to the top of the sample of the product that is inside the centrifuge tube. Slowly push the plunger while withdrawing the syringe from the centrifuge tube. Check for air bubbles, and eliminate them by tapping down the centrifuge tube. Fill the centrifuge tube to its maximum capacity with the sample of the product (i.e. all the way to the rim), cap the centrifuge tube and place in the centrifuge tube rack. Repeat these steps until all 24 centrifuge tubes are filled.

Load the centrifuge as described in the manufacturer's instrument operation section of the instruction manual. Centrifuge each of the samples for 15 minutes at 13,000 rpm. Once centrifugation is done, remove each centrifuge tube from centrifuge. Next, use a caliper to measure the length of benefit phase to 1/100 of mm. Record the length of benefit phase for each sample.

FIG. 2A is a diagram of the layers of a personal care composition after centrifugation. FIG. 2B and FIG. 2C are photographs that exemplify the measurement of the benefit phase comprising hydrophobic benefit material within in the centrifuged samples.

The volume of each dispensed sample is calculated by convert the weight of each sample to volume using product density (0.88 g/mL).

${Volume}_{({sample})} = \frac{Weight}{Density}$

The total volume dispensed is calculated by adding the volume of a sample to the sum of the volumes of all previous samples. The percent hydrophobic benefit material is calculated using equation of calibration curve, below. In this equation, y=length of benefit layer and x=the percentage hydrophobic benefit material in the sample.

$X = \frac{y + 3.0416}{0.3867}$

FIG. 3 depicts a calibration curve that was generated from 20 to 70% concentration of hydrophobic benefit material. This curve was used to transform mm of hydrophobic benefit material to percent of hydrophobic benefit material in the composition.

Finally, plot the percentage of hydrophobic benefit material versus the total volume dispensed to obtain the hydrophobic benefit material distribution profile of the personal care article throughout the package.

Magnetic Resonance Imaging (MRI) Method:

The MRI Method is used to obtain images and quantitatively describe the benefit distribution in 3-Dimension. The Instrument used is a 4.7T Magnex Scientific magnet with a 60 cm horizontal bore. The data is collected using a Bruker 25 cm imaging coil and Bruker Paravision 3.0.2. The data is collected using a spin-echo pulse sequence, repetition time of 1000 ms and echo time of 15 ms.

Images were acquired of 32 of 2 mm thick slices were acquired along the flat surface of the package or bottle. The fields of view were 22 cm×10 cm with data size of 256×128, which results in in-plane pixel resolutions of 86 um×78 um.

The customized imaging analysis software used to analyze the MRI images is a Matlab based graphical user interface program, hereinafter referred to as “GUI program”. This GUI program was developed in order to quantitatively describe benefit layer distribution in 3-dimensions. The GUI program sets thresholds based on MRI intensity to segment background and/or void region, benefit region and surfactant region. The distribution of hydrophobic benefit material along the height and radial are summed and plotted as FIG. 4 and FIG. 5. FIG. 4 illustrates GUI based analysis of personal care composition phase distribution along the radial dimensions of the package. FIG. 5 illustrates GUI based analysis of personal care composition phase distribution along the height of the package.

Dynamic Shipping Stability Method:

The dynamic shipping stability method is a simulated shipping test that is conducted to illustrate the impact of the amount headspace on the distribution profile of hydrophobic benefit material in a personal care article used in accordance with the present invention. The method is conducted on a vibration table, such as a MTS Vibration Table, available from Lansmont TTV of Monterrey, Calif.

The method tests shipping cases of personal care articles. There are 6 personal care articles or packages that are comprised within a shipping case. The personal care articles are filled with inventive example B using inventive filler profile B with various headspaces at 16%, 10% and 3%, of the volume of the personal care article, respectively. The shipping cases are submitted to simulated shipping conditions. The temperature of the shipping cases of personal care articles can be varied to simulate shipping conditions from cold to warm climate regions.

Prior to submitting the shipping cases to simulated shipping conditions, MRI images of each personal care articled are obtained by the MRI method at 25° C. Next, the shipping cases are subjected to simulated shipping conditions

There are four steps to induce the simulated shipping conditions:

Step 1: The shipping cases are dropped once at each of the six orientations for a total of six times. The “six orientations,” of the shipping cases used are up, down, and on each of the four sides.

Step 2: The ASTM D4169 Truck Level 2 method is performed on the shipping cases in upright positions for three hours.

Step 3: The ASTM D4728 Truck method is performed with shipping cases at the six orientations for thirty minutes for each orientation.

Step 4: The shipping cases are dropped once at each of the six orientations for a total of six times.

After submitting the shipping cases to simulated shipping conditions, MRI images are taken for each personal care article by the MRI method at 25° C.

The MRI images prior to and after simulated shipping conditions are visually compared and graded of the shipping stability. The MRI images are compared on the amount of phase mixing, the presence of a zone of high concentration of hydrophobic benefit material, the orientation of the concentration of hydrophobic benefit material medial to the dispensing orifice, the amount of void volume and an orientation of the void volume at the end proximal to the dispensing orifice. If after submitting the shipping cases to simulated shipping conditions, the MRI images that show an excessive amount of mixing, the absence of a zone of high concentration of hydrophobic benefit material, an excessive amount of void volume and/or the volume is located medial or distal to the dispensing orifice; the personal care article would fail the dynamic stability shipping method. Conversely, if after submitting the shipping cases to simulated shipping conditions, the MRI images that show only a slight amount of mixing, the presence of a zone of high concentration of hydrophobic benefit material which is located medial to the dispensing orifice, a small amount of void volume located proximal to the dispensing orifice; the personal care article would pass the dynamic stability shipping method.

The results of the dynamic shipping stability method are shown below in FIG. 6A, FIG. 6B and FIG. 6C. As shown in FIG. 6A, the packages with 16% headspace shows extensive co-mixing of the two phases and thus, failed the shipping dynamic shipping stability method. As shown in FIG. 6B, the packages with 10% headspace shows improved dynamic shipping stability method as the zone of high concentration of hydrophobic benefit material is still apparent in the MRI image. As shown in FIG. 6C, the packages with 3% headspace shows the best shipping stability as the variable concentrations of hydrophobic benefit material is maintained after shipping protocol.

Ultracentrifugation Method:

The Ultracentrifugation Method is used to determine the percent of a structured domain or an opaque structured domain that is present in a personal care composition that comprises a surfactant phase or a surfactant component. The method involves the separation of a composition by ultracentrifugation into separate but distinguishable layers. The first personal care composition, second personal care composition and third personal care composition have multiple distinguishable layers, for example a non-structured surfactant layer, a structured surfactant layer, and a benefit layer.

First, dispense about 4 grams of personal care composition into Beckman Centrifuge Tube (11×60 mm). Next, place the centrifuge tubes in an Ultracentrifuge (Beckman Model L8-M or equivalent) and ultracentrifuge using the following conditions: 50,000 rpm, 18 hours, and 25° C.

After ultracentrifuging for 18 hours, determine the relative phase volume by measuring the height of each layer visually using an Electronic Digital Caliper (within 0.01 mm). First, the total height is measured as H_(a) which includes all materials in the ultracentrifuge tube. Second, the height of the benefit layer is measured as H_(b). Third, the structured surfactant layer is measured as H. The benefit layer is determined by its low moisture content (less than 10% water as measured by Karl Fischer Titration). It generally presents at the top of the centrifuge tube. The total surfactant layer height (H_(a)) can be calculated by this equation:

H _(s) =H _(a) −H _(b)

The structured surfactant layer components may comprise several layers or a single layer. Upon ultracentrifugation, there is generally an isotropic layer at the bottom or next to the bottom of the ultracentrifuge tube. This clear isotropic layer typically represents the non-structured micellar surfactant layer. The layers above the isotropic phase generally comprise higher surfactant concentration with higher ordered structures (such as liquid crystals). These structured layers are sometimes opaque to naked eyes, or translucent, or clear. There is generally a distinct phase boundary between the structured layer and the non-structured isotropic layer. The physical nature of the structured surfactant layers can be determined through microscopy under polarized light. The structured surfactant layers typically exhibit distinctive texture under polarized light. Another method for characterizing the structured surfactant layer is to use X-ray diffraction technique. Structured surfactant layer display multiple lines that are often associated primarily with the long spacings of the liquid crystal structure. There may be several structured layers present, so that H_(c) is the sum of the individual structured layers. If a coacervate phase or any type of polymer-surfactant phase is present, it is considered a structured phase.

Finally, the structured domain volume ratio is calculated as follows:

Structured Domain Volume Ratio=H _(c) /H _(s)*100%

If there is no benefit phase present, use the total height as the surfactant layer height, H_(s)=H_(a).

Yield Stress and Zero Shear Viscosity Method:

The Yield Stress and Zero Shear Viscosity of a composition contained within a zone, can be measured either prior to combining the phases in a composition, or after combining the phases in a composition by separating the phases by suitable physical separation means, such as centrifugation, pipetting, cutting away mechanically, rinsing, filtering, or other separation means. In the case of testing from a product package, two zones can be selected from the package that contains at least two compositions that contain separate hydrophobic benefit material concentrations. In order to separate the zones, the product can be frozen at a temperature of at least −20° C. for a period of at least 24 hours. The zones are then cut using a cutting implement such as a bandsaw. The cut portions are collected separately and allowed equilibrate to ambient conditions.

A controlled stress rheometer, such as a TA Instruments AR2000 Rheometer, is used to determine the Yield Stress and Zero Shear Viscosity. The determination is performed at 25° C. with the 4 cm diameter parallel plate measuring system and a 1 mm gap. The geometry has a shear stress factor of 79580 m⁻³ to convert torque obtained to stress. Serrated plates can be used to obtain consistent results when slip occurs.

First a sample of the composition is obtained and placed in position on the rheometer base plate, the measurement geometry (upper plate) moving into position 1 mm above the base plate. Excess phase at the geometry edge is removed by scraping after locking the geometry. If the phase comprises particles discernible to the eye or by feel (beads, e.g.) which are larger than about 150 microns in number average diameter, the gap setting between the base plate and upper plate is increased to the smaller of 4 mm or 8-fold the diameter of the 95^(th) volume percentile particle diameter. If a phase has any particle larger than 5 mm in any dimension, the particles are removed prior to the measurement.

The determination is performed via the programmed application of a continuous shear stress ramp from 0.1 Pa to 1,000 Pa over a time interval of 4 minutes using a logarithmic progression, i.e., measurement points evenly spaced on a logarithmic scale. Thirty (30) measurement points per decade of stress increase are obtained. Stress, strain and viscosity are recorded. If the measurement result is incomplete, for example if material flows from the gap, results obtained are evaluated and incomplete data points excluded. The Yield Stress is determined as follows. Stress (Pa) and strain (unitless) data are transformed by taking their logarithms (base 10). Log(stress) is graphed vs. log(strain) for only the data obtained between a stress of 0.2 Pa and 2.0 Pa, about 30 points. If the viscosity at a stress of 1 Pa is less than 500 Pa-sec but greater than 75 Pa-sec, then log(stress) is graphed vs. log(strain) for only the data between 0.2 Pa and 1.0 Pa, and the following mathematical procedure is followed. If the viscosity at a stress of 1 Pa is less than 75 Pa-sec, the zero shear viscosity is the median of the 4 highest viscosity values (i.e., individual points) obtained in the test, the yield stress is zero, and the following mathematical procedure is not used. The mathematical procedure is as follows. A straight line least squares regression is performed on the results using the logarithmically transformed data in the indicated stress region, an equation being obtained of the form:

Log(strain)=m*Log(stress)+b  (1)

Using the regression obtained, for each stress value (i.e., individual point) in the determination between 0.1 and 1,000 Pa, a predicted value of log(strain) is obtained using the coefficients m and b obtained, and the actual stress, using Equation (1). From the predicted log(strain), a predicted strain at each stress is obtained by taking the antilog (i.e., 10^(x) for each x). The predicted strain is compared to the actual strain at each measurement point to obtain a % variation at each point, using Equation (2).

%variation=100*(measured strain−predicted strain)/measured strain  (2)

The Yield Stress is the first stress (Pa) at which % variation exceeds 10% and subsequent (higher) stresses result in even greater variation than 10% due to the onset of flow or deformation of the structure. The Zero Shear Viscosity is obtained by taking a first median value of viscosity in Pascal-seconds (Pa-sec) for viscosity data obtained between and including 0.1 Pa and the Yield Stress. After taking the first median viscosity, all viscosity values greater than 5-fold the first median value and less than 0.2× the median value are excluded, and a second median viscosity value is obtained of the same viscosity data, excluding the indicated data points. The second median viscosity so obtained is the Zero Shear Viscosity.

VI. Method of Manufacture

In one embodiment, the personal care articles of the present invention are manufactured by a dual phase filler. The dual phase filler is associated with storage vessels, a combiner, a blender and nozzle for filling multiple personal care compositions. An example of a dual phase filler and associated software is manufactured by Antonio Mengibar Packaging Machinery of Barcelona, Spain. The surfactant phase and benefit phase of the personal care compositions are stored in separate storage vessel; each vessel equipped with a pump and a hose assembly. A programmed filler profile of the dual-phase filler controls the pumping of specific ratios of the two phases of the personal care compositions which result in the zones within a package. The two phases of the personal care compositions are pumped from the storage tanks into a combiner where the two phases are combined. After the phases are combined; they are mixed in a blender. From the blender, the resultant product is pumped via a hose into a single nozzle. The nozzle is placed into a container and fills a product package with a single resulting product. In some embodiments, the resultant product exhibits a distinct pattern of the phases which are visually distinct. In other embodiments, the resultant product exhibits a uniform appearance without a pattern. If a pattern is present, the pattern is selected from the group consisting of striped, marbled, geometric, and combinations thereof.

In another embodiment, the personal care compositions used in accordance with the present invention are manufactured according to the method disclosed in U.S. patent application Ser. No. 10/837,214 Publication No. 2004/0219119 A1 entitled “Visually distinctive multiple liquid phase compositions” filed by Wei et al. on Apr. 30, 2004, published on Nov. 18, 2004. Alternatively, it may be effective to combine toothpaste-tube filling technology with a spinning stage design. In still another embodiment, the personal care compositions are prepared by the method and apparatus as disclosed in U.S. Pat. No. 6,213,166 issued to Thibiant et al. on Apr. 10, 2001. The method and apparatus allow two or more compositions to be filled with a spiral configuration into a single product package. The method requires that at least two nozzles be employed to fill the compositions into a package. The package is placed on a moving stage and spun as the composition is introduced into the package.

Non-limiting examples of the personal care compositions, ratios of phases and filler profiles are disclosed in the examples below.

VII. Composition and Articles Examples Example 1 Exemplary Personal Care Articles

Table 2 shows non-limiting examples of the personal care articles of the present invention and a comparative example. These personal care articles are made and filled in a single chamber package. The personal care compositions used in accordance with the present invention comprise various concentrations of hydrophobic benefit material through out the package. These personal care compositions used in accordance with the present invention are filled in a package within multiples zones. The comparative example comprises uniform concentration of hydrophobic benefit material through out the package.

TABLE 2 Examples of the Present Invention and Comparative Example Inventive Inventive Comparative Example A Example B Example C Surfactant Phase Composition Sodium Lauroamphoacetate^(1.) 4.9 4.9 4.9 Sodium Trideceth Sulfate^(2.) 8.4 8.4 8.4 Sodium Lauryl Sulfate 8.4 8.4 8.4 Trideceth-3^(3.) 2.0 2.0 2.0 Sodium Chloride 4.75 4.75 4.75 Guar 0.6 0.6 0.6 hydroxypropyltrimonium chloride^(4.) Polyethyleneoxide^(5.) 0.15 0.15 0.15 Xanthan gum^(6.) 0.2 0.2 0.2 Hollow microspheres^(7.) 0.36 0.3 0.3 Methyl chloro isothiazolinone 0.0005 0.0005 0.0005 and methyl isothiazolinone^(8.) EDTA^(9.) 0.15 0.15 0.15 Sodium Benzoate 0.2 0.2 0.2 Citric Acid, titrate pH = pH = pH = 5.7 ± 0.2 5.7 ± 0.2 5.7 ± 0.2 Perfume 1.3 1.3 1.3 Water Q.S. Q.S. Q.S. Benefit Phase Composition Petrolatum ^(10.) 70 70 70 Mineral Oil^(11.) 30 30 30 Filler Profile Inventive Inventive Comparative Profile A Profile B Profile C ^(1.)available from Cognis Chemical Corp. ^(2.)sulfanated to >95% sulfate from ICONOL ® TDA-3 available from BASF Corp., ^(3.)ICONOL ® TDA-3 available from BASF Corp., ^(4.)N-HANCE ® 3196 Polymer from Aqualon of Wilmington, DE, ^(5.)POLYOX ™ WSR-301 available from DOW ® Chemical Corp., ^(6.)KELTRO ™ 1000 available from CP Kelco, ^(7.)EXPANCEL ® microspheres available from 091 WE40 d24, Akzo Nobel, ^(8.)KATHON ® CG available for Rohm & Haas, ^(9.)DISSOLVINE ® NA 2x available from Akzo Nobel, ^(10.)G2218 petrolatum from Sonneborn, ^(11.)HYDROBRITE ® 1000 White Mineral Oil available from Sonneborn.

The compositions described above can be prepared by conventional formulation and mixing techniques. The surfactant phase composition is made by first preparing a citric acid premix and then a polymer pre-mix. The citric acid premix is prepared by adding citric acid into water at a ratio of 1:3. The polymer premix is prepared by adding polyethyleneoxide and xanthan gum into trideceth-3. The following ingredients are then added into the main mixing vessel in the following sequence with agitation: water, guar hydroxypropyltrimonium chloride, hollow microspheres, sodium lauroamphoacetate, sodium trideceth sulfate, sodium lauryl sulfate, sodium chloride, sodium benzoate, and disodium EDTA. The citric acid premix is added into the main mixing vessel and the pH of the composition is adjusted to 5.7±0.2. The polymer premix is next added into the main mixing vessel with continuous agitation. Perfume and methyl chloro isothiazolinone and methyl isothiazolinone are added while continuing the agitation until the composition is homogeneous. The resultant surfactant phase composition is fed into the dual-phase filler through a hose-assembly.

The benefit phase composition is prepared by first adding petrolatum into a mixing vessel. The mixing vessel has been heated to 82.2° C. Mineral oil is added into the mixing vessel with agitation. The benefit phase composition is cooled to 44° C. through a scraped-wall heat-exchanger, such as that manufactured by Waukesha Cherry-Burrell, Delavan, Wis. After cooling, the resultant benefit phase composition is fed into the dual-phase filler through a second hose-assembly.

The filler profiles A, B and C are examples of filling programs that specify the ratios of the surfactant and benefit phases within packages filled by a dual phase filler. Filler profiles A and B specify variable hydrophobic benefit material concentrations throughout the zones of the personal care articles of the present invention. Whereas filler profile C specifies uniform hydrophobic benefit material concentrations in the resultant personal care article within the package.

TABLE 3 Dual Phase Filler Profiles for Example A and B Filler Profile A Filler Profile B Benefit Sur- Benefit Sur- Dose Material factant Dose Material factant Step (mL) % % Step (mL) % % 1 33.6 24 76 1 33.2 30 70 2 61.4 42 58 2 61.7 50 50 3 70.6 52 48 3 71.2 60 40 4 104.2 63 37 4 104.4 70 30 5 133.2 63 37 5 132.9 60 40 6 155.2 52 48 6 154.7 50 50 7 174.9 42 58 7 194.6 40 60 8 194.5 32 68 8 223.1 20 80 9 223.5 15 85 9 248.7 10 90 10 249.0 7 93 10 280.0 20 80 11 280.2 15 85 11 289.5 30 70 12 289.5 27 73 — — — —

TABLE 4 Dual Phase Filler Profiles for Example C Filler Profile C Step Dose (mL) Benefit Material % Surfactant % 1 11 45 55 2 20 45 55 3 35 45 55 4 52 45 55 5 75 45 55 6 108 45 55 7 148 45 55 8 188 45 55 9 229 45 55 10 265 45 55 11 280 45 55

FIG. 7 depicts MRI images that illustrate the surfactant and hydrophobic benefit material distribution in a package of examples A, B and C. These images were taken by the MRI Method, described in detail in the Test Methods above. As shown in FIG. 7, the comparative example C shows a uniform hydrophobic benefit material distribution throughout the package. Inventive examples A and B, in FIG. 7 show a variable hydrophobic benefit material distribution profile with higher benefit zones are highlighted with arrows.

FIG. 8 is a chart of the hydrophobic benefit material distribution in examples A and B of the present invention. The Micro centrifugation Method, described in detail in the Test Methods above, was used to quantify the hydrophobic benefit material distribution in the inventive examples A and B. Profile A and profile B, shown in FIG. 8 clearly show a variable benefit distribution from the beginning, middle, and end of the dispensing.

The dimensions and values disclosed herein are not to be understood as being strictly limited to the exact numerical values recited. Instead, unless otherwise specified, each such dimension is intended to mean both the recited value and a functionally equivalent range surrounding that value. For example, a dimension disclosed as “40 mm” is intended to mean “about 40 mm.”

All documents cited in the Detailed Description of the Invention are, in relevant part, incorporated herein by reference; the citation of any document is not to be construed as an admission that it is prior art with respect to the present invention. To the extent that any meaning or definition of a term in this document conflicts with any meaning or definition of the same term in a document incorporated by reference, the meaning or definition assigned to that term in this document shall govern.

While particular embodiments of the present invention have been illustrated and described, it would be obvious to those skilled in the art that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention. 

1. A method for identifying a formulation comprising a hydrophobic benefit agent useful for improving the skin (stratum corneum barrier) in a human subject, comprising: generating one or more negative skin profiles for a human subject having dry or damaged skin; contacting the skin of the human subject with a proposed rinse-off personal care formulation generating one or more test profiles comparing the one or more test profiles to the one or more negative profiles and identifying the proposed formulation as effective if the test profile is directionally shifted away from the negative reference profile and shows at least one skin property selected from (i) reduction of visual dryness, a reduction in trans-epidermal water loss, increased skin hydration, increased elastic extension, increased elastic recovery, increased firmness and (ii) reduction in total protein, an increase in the amount of one or more of Keratin 1, Keratin 10 and Keratin 11, and a decrease in cytokine expression.
 2. A rinse-off personal skin care composition effective for improving one or both of stratum corneum barrier maintenance and repair properties in aged skin, comprising a formulation identified according to the method of claim
 1. 3. A method for improving one or both of stratum corneum barrier maintenance and repair properties, comprising contacting skin with the formulation identified according to the method of claim
 1. 4. The method according to claim 1, wherein the measurable improvement is a reduction of visual dryness, wherein the visual dryness reduction is greater than 0.5 dryness unit vs. water control after 3 hours of product application.
 5. The method according to claim 1, wherein the measurable improvement is a reduction in trans-epidermal water loss, wherein the reduction of trans-epidermal water loss is greater than 0.2 TEWL unit vs. water control after 3 hours of product application.
 6. The method according to claim 1, wherein the measurable improvement is increased skin hydration, wherein the increased skin hydration is greater than one Corneometer Unit vs. water control after 3 hours of product application.
 7. The method according to claim 1, wherein the measurable improvement is increased elastic extension, wherein the elastic extension improvement index is greater than 5 after one hour of product application.
 8. The method according to claim 1, wherein the measurable improvement is increased elastic recovery, wherein the elastic recovery improvement index is greater than 5 after one hour of product application.
 9. The method according to claim 1, wherein the measurable improvement is increased firmness, wherein the skin firmness improvement index is greater than 4 after one of product application.
 10. The method according to claim 1, wherein the measurable improvement is reduction in total protein, wherein the total protein improvement index is greater than
 10. 11. The method according to claim 1, wherein the measurable improvement is an increase in the amount of one or more of Keratin 1, Keratin 10 and Keratin 11, wherein the Keratin improvement index is greater than
 50. 